7890A Manual

Agilent 7890A Gas Chromatograph
Advanced User Guide
Agilent Technologies
Notices
Agilent Technologies, Inc. 2009 No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws.
Safety Notices CAUTION

A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.
Manual Part Number

G3430-90015
Edition
Fourth edition, April 2009 Third edition, September 2008 Second edition, January 2008 First edition, April 2007 Printed in USA Agilent Technologies, Inc. 2850 Centerville Road Wilmington, DE 19808-1610 USA 412 800820 3278
WA R N I N G
A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met.
Contents
1 Programming
Run Time Programming 16 Using run time events 16 Programming run time events The run table 17 Adding events to the run table Editing events in the run table Deleting run time events 18 Clock Time Programming 19 Using clock time events 19 Programming clock time events Adding events to the clock table Editing clock time events 20 Deleting clock time events 20
17 17 17
19 19
User-Key Programming 21 To program a User Key 21 To play back (execute) the stored keystrokes To erase the stored keystrokes 21
21
Configuration
About Configuration 24 Assigning GC resources to a device 24 Setting configuration properties 25 General Topics 26 Unlock the GC Configuration Ignore Ready = 26 Information displays 26 Unconfigured: 27 26
Oven 28 To configure the oven 28 To configure the oven for cryogenic cooling Front Inlet/Back Inlet 30 To configure the Gas type 30 To configure the MMI, PTV or COC coolant Column # 32 To configure a single column 32 To configure multiple columns 34
29
30
Advanced User Guide
Cryo Trap 40 Configure the cryo trap to the GC 40 Configure a heater to the cryo trap 40 Configure the coolant 40 Configure the user-configurable heater 41 Reboot the GC 41 Front Detector/Back Detector/Aux Detector/Aux Detector 2 To configure the makeup/reference gas 42 Lit offset 42 To configure the FPD heaters 42 Analog out 1/Analog out 2 Fast peaks 43 43 42
Valve Box 44 To assign a GC power source to a valve box heater Thermal Aux 45 To assign a GC power source to an Aux thermal zone To configure an MSD transfer line heater 45 To configure a nickel catalyst heater 46 To configure an AED transfer line heater 46 PCM A/PCM B/PCM C 47 To assign a GC communication source to a PCM To configure a PCM 47
44 45
47
Pressure aux 1,2,3/Pressure aux 4,5,6/Pressure aux 7,8,9 49 To assign a GC communication source to an Aux EPC 49 To configure an auxiliary pressure channel 49 Status 50 The Ready/Not Ready status table 50 The setpoint status table 50 To configure the setpoint status table 50 Time 51 To set time and date 51 To use the stopwatch 51 Valve # 52 To configure a valve 52
Front injector/Back injector 53 Solvent Wash Mode (7683 ALS) 53 To configure an injector (7683 ALS) 54 Sample tray (7683 ALS) Instrument 56 55
Advanced User Guide
Options
About Options 58 59
Calibration 59 Maintaining EPC calibrationinlets, detectors, PCM, and AUX To zero all pressure sensors in all modules 61 Column calibration 61 Communication 65 Configuring the IP address for the GC Keyboard and Display 66 65
Chromatographic Checkout
About Chromatographic Checkout 70 71
To Prepare for Chromatographic Checkout To Check FID Performance To Check TCD Performance To Check NPD Performance To Check uECD Performance 73 78 83 88
To Check FPD Performance (Sample 5188-5953) To Verify FPD Performance (Sample 5188-5245)
93 101
Methods and Sequences

Creating Methods 110 To program a method 111 To program the ALS 111 To program the ALS sampler tray 111 To program the 7683B ALS bar code reader To save a method 113 To load a stored method 113 Method mismatch 114 Creating Sequences 115 About the priority sequence 115 To program a sequence 116 To program a priority sequence 116 To program an ALS subsequence 117 To program a valve subsequence 117 To program post sequence events 117 To save a sequence 118 To load a stored sequence 118 To determine sequence status 118
112
Advanced User Guide
To start a sequence 118 To pause and resume a sequence To stop a sequence 119 To abort a sequence 119
119
Checking for Leaks

Preparing the GC for Maintenance 122 Column and oven preparation 122 Inlet preparation 122 Detector preparation 122 Leak Check Tips 123 124
To Check for External Leaks To Check for GC Leaks 125
Leaks in Capillary Column (Microfluidic) Fittings To Perform a SS Inlet Pressure Decay Test To Correct Leaks in the Split Splitless Inlet 127 131
126
To Perform a Multimode Inlet Pressure Decay Test To Correct Leaks in the Multimode Inlet To Perform a PP Inlet Pressure Decay Test To Correct Leaks in the Packed Column Inlet To Perform a COC Pressure Decay Test 142 145 136 137 141
132
To Correct Leaks in the Cool On-Column Inlet To Perform a PTV Pressure Decay Test To Correct Leaks in the PTV Inlet 150 151 146
To Perform a VI Pressure Decay Test
To Prepare the VI for a Closed System Leak Check To Correct Leaks in the Volatiles Interface 156
155
Flow and Pressure Modules

About Flow and Pressure Control Maximum operating pressure PIDs 159 Inlet Modules 160 161 162 165 158 158
Detector Modules
Pressure Control Modules
Auxiliary Pressure Controllers
Advanced User Guide
Restrictors
166 167
Examples 167 1. Using an Aux epc channel to supply purge gas to a splitter 2. Using the PCM channels 167
Inlets
Using Hydrogen Inlet Overview 171 172 173
Carrier Gas Flow Rates
About Gas Saver 174 To use gas saver 174 Pre Run and Prep Run 176 The [Prep Run] key 176 Auto Prep Run 177 About Heaters 178
About the Split/Splitless Inlet 180 Septum tightening (S/SL) 180 Standard and high-pressure versions of the S/SL inlet 180 Split/Splitless inlet split mode overview 181 Split/Splitless inlet splitless mode overview 182 The S/SL inlet pulsed split and splitless modes 183 Split/Splitless inlet split mode minimum operating pressures Selecting the correct S/SL inlet liner 185 Vapor Volume Calculator 187 Setting parameters for the S/SL split mode 187 Selecting parameters for the S/SL splitless mode 188 Setting parameters for the S/SL splitless mode 189 Setting parameters for the S/SL pulsed modes 190 About the Multimode Inlet 191 Septum tightening (MMI) 191 Heating the MMI 192 Cooling the MMI 192 MMI split mode minimum operating pressures 193 Selecting the correct MMI liner 194 Vapor Volume Calculator 195 MMI split and pulsed split modes 195 MMI splitless and pulsed splitless modes 199 MMI solvent vent mode 205 MMI Direct Mode 213 To develop a MMI method that uses large volume injection
184
214
Advanced User Guide
Multiple injections with the MMI About the Packed Column Inlet Setting parameters 225 About the Packed Column Inlet Setting parameters 229 223 227
217
About the Cool On-Column Inlet 231 Setup modes of the COC inlet 232 Retention gaps 232 COC inlet temperature control 232 Setting COC inlet flows/pressures 233 Setting COC inlet parameters 233 About the PTV Inlet 235 PTV sampling heads 235 Heating the PTV inlet 236 Cooling the PTV inlet 237 PTV inlet split and pulsed split modes 237 PTV inlet splitless and pulsed splitless modes 241 PTV inlet solvent vent mode 248 To develop a PTV method that uses large volume injection Multiple injections with the PTV inlet 259 About the Volatiles Interface 265 VI operating modes 266 About the VI split mode 267 About the VI splitless mode 271 About the VI direct mode 276 Preparing the Interface for Direct Sample Introduction Disconnecting the split vent line 279 Configuring for direct mode 281 VI direct mode setpoint dependencies 281 VI direct mode initial values 282 Setting parameters for the VI direct mode 282 279
256
Columns and Oven

About the Oven Oven safety 286 286 287
Configuring the Oven
Cryogenic Operation 288 Cryogenic setpoints 288 About Oven Temperature Programming Programming setpoints 290 290
Advanced User Guide
Post run 291 Oven ramp rates 291 Setting the oven parameters for constant temperature 292 Setting the oven parameters for ramped temperature 292 About the Oven Insert 294
About Columns 295 Selecting the correct packed glass column type 295 About the column modes 295 Select a column mode 296 Setting the column parameters for constant flow or constant pressure 297 Enter a flow or pressure program (optional) 297 Programming column pressure or flow 298 Backflushing a Column 299 Backflushing when connected to an MSD 299 Backflushing using a capillary flow technology device Nickel Catalyst Tube 305 About the nickel catalyst tube 305 Gas flows 305 Setting temperatures for the nickel catalyst tube
300
306
10
Detectors
About Makeup Gas 308 310
About the FID 309 How FID units are displayed in Agilent data systems and on the GC To light the FID flame 311 To extinguish the FID flame 311 FID automatic reignition (Lit offset) 311 Recommended starting conditions for new FID methods 312 Setting parameters for FID 313 About the TCD 314 TCD pneumatics 316 TCD carrier, reference, and makeup gas 316 TCD gas pressures 317 Selecting reference and makeup flows for the TCD 318 Chemically active compounds reduce TCD filament life 318 Changing the TCD polarity during a run 319 Detecting hydrogen with the TCD using helium carrier gas 319 Setting parameters for the TCD 320 About the uECD 322 uECD safety and regulatory information 322
Advanced User Guide
uECD warnings 323 Safety precautions when handling uECDs 325 uECD gas flows 326 uECD linearity 326 uECD detector gas 326 uECD temperature 326 uECD analog output 327 Recommended starting conditions for new uECD methods uECD makeup gas notes 327 uECD temperature programming 328 Setting parameters for the uECD 328 About the NPD 329 New NPD features and changes 329 NPD software requirements 329 NPD flows and general information 329 NPD flow, temperature, and bead recommendations NPD required gas purity 332 Setting parameters for the NPD 333 Selecting an NPD bead type 334 Changing from a ceramic bead to a Blos bead 335 Selecting an NPD jet 335 To configure the NPD 337 Automatically adjusting NPD bead voltage 338 Setting NPD adjust offset on the clock table 339 Aborting NPD adjust offset 339 Extending the NPD bead life 339 Setting the initial bead voltage for new beads 340 Setting NPD bead voltage manually (optional) 340 About the FPD 342 FPD linearity 343 FPD Lit Offset 343 Starting Up and Shutting Down the FPD FPD photomultiplier protection 343 FPD optical filters 343 Inlet liners for use with the FPD 344 FPD temperature considerations 344 FPD gas purity 344 FPD gas flows 344 Lighting the FPD flame 345 Setting parameters for the FPD 346
327
330
343
10
Advanced User Guide
11
Valves
About Valves 350
The Valve Box 351 Heating the valves 351 Valve temperature programming Configuring an Aux thermal zone Valve Control 353 The valve drivers 353 The internal valve drivers The external valve drivers Valve Types 355 356
352 352
353 354
Configuring a Valve
Controlling a Valve 357 From the keyboard 357 From the run or clock time tables 357 Simple valve: column selection 357 Gas sampling valve 358 Multiposition stream selection valve with sampling valve
359
12
7683B Sampler
About the 7683B Sampler Hardware 362 Software 362 362
Setting Parameters for the ALS 363 Solvent Saver 364 Sample tray setpoints 365 Storing setpoints 365
13
Cables
About Cables and Back Panel Connectors Back panel connectors 368 Sampler connectors 368 The AUX connector 368 Signal connectors 369 REMOTE connector 369 EVENT connector 369 BCD input connector 369 RS-232 connector 369 LAN connector 369 Using the Remote Start/Stop cable 370 368
Advanced User Guide
11
Connecting Agilent products 370 Connecting non-Agilent products 370 Connecting Cables 373
Cable Diagrams 375 Analog cable, general use 375 Remote start/stop cable 375 BCD cable 376 External event cable 377
14
GC Output Signals
About Signals 380
Signal Types 381 Value 381 Analog Signals 383 Analog zero 383 Analog range 383 Analog data rates 384 Selecting fast peaks (analog output) Digital Signals 386 Digital zero 386 Baseline level shifts 386 Agilent data systems 387 Zero Init Data Files 389 Column Compensation 390 Creating a column compensation profile 391 Making a run using analog output column compensation Making a run using digital output column compensation Plotting a stored column compensation profile 392 Test Plot 393
385
391 391
15
Miscellaneous Topics
Auxiliary Devices 396 About Auxiliary Pressure Control 396 About Aux Thermal Zone Control 397 About Auxiliary Device Contacts 397 About the 24V Auxiliary Device Power Supply About Auxiliary Columns 397 About Auxiliary Detectors 398 To Use the Stopwatch Service Mode 400 399
397
12
Advanced User Guide
Service Reminders 400 Other functions 401
Advanced User Guide
13
14
Advanced User Guide
Agilent 7890A Gas Chromatograph Advanced User Guide
1 Programming
Run Time Programming 16 Using run time events 16 Programming run time events 17 The run table 17 Adding events to the run table 17 Editing events in the run table 17 Deleting run time events 18 Clock Time Programming 19 Using clock time events 19 Programming clock time events 19 Adding events to the clock table 19 Editing clock time events 20 Deleting clock time events 20 User-Key Programming 21 To play back (execute) the stored keystrokes 21 To erase the stored keystrokes 21 To program a User Key 21
15
Run Time Programming

Run time programming allows certain setpoints to change automatically during a run as a function of the chromatographic run time. Thus an event that is programmed to occur at 2 minutes will occur 2 minutes after every injection. Its uses include: Controlling column switching or other valves Changing signal definition, zero, or range Controlling an auxiliary pressure channel Changing polarity of a thermal conductivity detector (TCD) Turning the hydrogen flow to a nitrogen- phosphorus detector (NPD) on or off Pausing (freezing) and resuming a signal value The changes are entered into a run table that specifies the setpoint to be changed, the time for the change, and the new value. At the end of the chromatographic run, most setpoints changed by a run time table are returned to their original values. Valves can be run time programmed but are not restored to their starting position at the end of the run. You must program the reset operation in the run table if this action is desired. See From the run or clock time tables on page 357.
Using run time events

The [Run Table] key is used to program timed events. You can control the following events during a run. Valves (1- 8) Multiposition valve Signal type (see Signal Types on page 381) Analog signal zero and range Digital signal zero and baseline level shifts (see Digital zero on page 386) Auxiliary pressures (1 through 9) TCD negative polarity (on/off) NPD H2 flow (on/off) Pausing (freezing) and resuming a signal value
16
Advanced User Guide
Programming run time events

1 Press [Run Table]. 2 Press [Mode/Type] to see the available run time events. 3 Scroll to the event to be programmed. Press [Enter]. 4 Enter values for the Time: and the other parameter. Press
[Enter] after each entry.

5 Press [Mode/Type] to add another event. Press [Status] to
terminate entries.
The run table

The programmed events are arranged in order of execution time in the Run Table. This is a brief example: RUN TABLE (1 of 3) Time: 0.10 Valve #2 On RUN TABLE (2 of 3) Time: 3 Analog signal 2 range 2 RUN TABLE (3 of 3) Time: 4.20 Valve #2 Off Event 1 rotates a valve.
Event 2 adjusts the signal range. Event 3 resets Valve #2 to its original position in preparation for another run. Valves do not reset automatically.
Adding events to the run table

1 To add new events to the run table, press [Mode/Type]
while on the Time: line of any entry.

2 Select the event type. 3 Set appropriate Time: and other parameters. Some require
numbers; others require [On/Yes] or [Off/No].

4 Repeat until all entries are added. Events are
automatically placed in order by execution time.
Editing events in the run table

1 Press [Run Table]. 2 Move the cursor to the event you want to change. 3 To edit the time for an event, move the cursor to the line
labeled Time:. Type the desired time and press [Enter].

4 To edit a setpoint value, scroll to the setpoint line. Press
[On/Yes] or [Off/No] or enter a numeric value for the setpoint. Press [Enter].
Advanced User Guide
17
Deleting run time events

1 Press [Run Table]. 2 From within this table press [Delete] to delete events from
the run time table. You will be asked to confirm the deletion.
3 Press [On/Yes] to delete the current timed event; press
[Off/No] to cancel this operation.

4 To delete the entire table, press [Delete][Run Table].
18
Advanced User Guide
Clock Time Programming

Clock time programming allows certain setpoints to change automatically at a specified time during a 24- hour day. Thus, an event programmed to occur at 14:35 hours will occur at 2:35 in the afternoon. A running analysis or sequence has precedence over any clock table events occurring during this time. Such events are not executed. Possible clock time events include: Valve control Method and sequence loading Starting sequences Initiating blank and prep runs Column compensation changes Adjustments of the detector offset
Using clock time events

The Clock Table function allows you to program events to occur during a day based on the 24- hour clock. Clock table events that would occur during a run or sequence are ignored. For example, the clock table could be used to make a blank run before you even get to work in the morning.
Programming clock time events

1 Press [Clock Table]. 2 Press [Mode/Type] to see the available clock time events. 3 Scroll to the parameter to be programmed. 4 Edit Time: and the setpoints for this event. 5 Press [Mode/Type] to add another event. Press [Status] to
terminate entries. When the clock event is executed, a confirming message appears.
Adding events to the clock table

1 Press [Clock Table]. 2 Press [Mode/Type]. When entries are added, they are
automatically ordered chronologically.

3 Select the event type.
Advanced User Guide
19
4 Set appropriate parameters. 5 Repeat this process until all entries are added.
Editing clock time events

1 Press [Clock Table] to view all events programmed. 2 Scroll to the event you want to change. 3 To edit the time for an event, move the cursor to the line
labelled Time: and type the desired time.

4 To edit a setpoint value, scroll to the setpoint item. Press
[On/Yes] or [Off/No], or enter a numerical value for the setpoint.
Deleting clock time events

1 Press [Clock Table]. 2 Use [Delete] to remove events from the clock time table.
You will be asked to confirm the deletion.

3 Press [On/Yes] to delete the current timed event; press
[Off/No] to cancel this operation. To delete the entire table, press [Delete][Clock Table].
20
Advanced User Guide
User-Key Programming
The two User Keys create macros (sets of frequently used keystrokes) and assign them to single keys. A macro is executed when the User Key is pressed. The stored keystrokes may be any keys except [Start], [Prog], [User Key 1], or [User Key 2]. This discussion assumes that you wish to program [User Key 1]. The process is the same for [User Key 2].
To program a User Key

1 Press [Prog]. Press [User Key 1]. 2 Press up to 31 keys, then press [User Key 1]. The
keystrokes are stored.
To play back (execute) the stored keystrokes

Press [User Key 1].
To erase the stored keystrokes

Press [Prog][User Key 1][User Key 1]. This creates an empty macro.
Advanced User Guide
21
22
Advanced User Guide
2 Configuration
About Configuration 24 Assigning GC resources to a device 24 Setting configuration properties 25 General Topics 26 Unlock the GC Configuration 26 Ignore Ready = 26 Information displays 26 Unconfigured: 27 Oven 28 Front Inlet/Back Inlet 30 To configure the MMI, PTV or COC coolant 30 Column # 32 To configure a single column 32 To configure multiple columns 34 Cryo Trap 40 Front Detector/Back Detector/Aux Detector/Aux Detector 2 42 Lit offset 42 To configure the FPD heaters 42 Analog out 1/Analog out 2 43 Fast peaks 43 Valve Box 44 Thermal Aux 45 To configure an MSD transfer line heater 45 To configure a nickel catalyst heater 46 To configure an AED transfer line heater 46 PCM A/PCM B/PCM C 47 Pressure aux 1,2,3/Pressure aux 4,5,6/Pressure aux 7,8,9 49 Status 50 The Ready/Not Ready status table 50 The setpoint status table 50 Time 51 Valve # 52 Front injector/Back injector 53 Sample tray (7683 ALS) 55 Instrument 56
23
Configuration
About Configuration
Configuration is a two- part process for most GC accessory devices that require power and/or communication resources from the GC. In the first part of the configuration process, a power and/or communication resource is assigned to the device. The second part of the configuration process allows setting of any configuration properties associated with the device.
Assigning GC resources to a device

A hardware device requiring but not assigned GC resources is given a mode of Unconfigured by the GC. Once you assign GC resources to a device, the GC gives the device a mode of Configured, allowing you to access other property settings (if any) for the device. To assign GC resources to a device with an Unconfigured mode:
1 Unlock the GC configuration. Press [Options], select
Keyboard & Display and press [Enter]. Scroll down to Hard Configuration Lock and press [Off/No].
2 Press [Config] on the GC keypad and select a device from
the list, then press [Enter]. The [Config] key opens a menu similar to this: Oven Front inlet Back Inlet Column # Front detector Back detector Aux detector Aux detector 2 Analog out 1 Analog out 2 Valve Box Thermal Aux 1 Thermal Aux 2 Thermal Aux 3 PCM A PCM B PCM C Aux EPC 1,2,3 Aux EPC 4,5,6
24
Advanced User Guide
Configuration
Aux EPC 7,8,9 Status Time Valve # 2 Dimensional GC Valve Front injector Back injector Sample tray Instrument In many cases you can move directly to the item of interest by pressing [Config][device].
3 When the Configure Device Display opens, the cursor
should be on the Unconfigured field. Press [Mode/Type] and follow the GC prompts to assign resources to the device.
4 After assigning resources, the GC prompts for you to
power cycle the GC. Turn the GC power switch off and then on. When the GC starts, select the device just assigned the GC resources for further configuration if needed. When accessed, its mode should indicate Configured and the other configuration properties are displayed.
Setting configuration properties

A devices configuration properties are constant for an instrument hardware setup unlike method settings which can change from sample run to sample run. An example of a configuration setting is the gas type flowing through a pneumatic device or the operation temperate limit of a device. To change the setting configuration properties for a Configured device:
1 Press [Config] on the GC keypad and select a device from
the list, then press [Enter]. In many cases you can move directly to the item of interest by pressing [Config][device].
2 Scroll to the device setting and change the property. This
can involve making a selection from a list using [Mode/Type], using [On/Yes] or [Off/No], or entering a numeric value. Press [Info] for help on changing numeric settings, or see the section of this document describing the specific configuration of the device.
Advanced User Guide
25
Configuration
General Topics
Unlock the GC Configuration
Accessory devices including inlets, detectors, pressure controllers (AUX EPC and PCM), and temperature control loops (Thermal AUX) have electrical connections to a power source and/or the communication bus in the GC. These devices must be assigned GC resources before they can be used. Before assigning resources to a device, you must first unlock the GC configuration. If you try to configure an Unconfigured device without unlocking the GC configuration, the GC displays the message CONFIGURATION IS LOCKED Go to Keyboard options to unlock. It is also necessary to unlock the GC configuration if you are removing the GC resources from a Configured device. This action returns the device state to Unconfigured. To unlock the GC configuration, press [Options], select Keyboard & Display and press [Enter]. Scroll down to Hard Configuration Lock and press [Off/No]. The GC configuration remains unlocked until the GC is power cycled off and on.
Ignore Ready =
The states of the various hardware elements are among the factors that determine whether the GC is Ready for analysis. Under some circumstances, you may not wish to have a specific element readiness considered in the GC readiness determination. This parameter lets you make that choice. For example, suppose an inlet heater is defective but you dont plan to use that inlet today. By setting Ignore Ready = TRUE for that inlet, you can use the rest of the GC. After the heater is repaired, set Ignore Ready = FALSE or the run could start before that inlets conditions are ready.
Information displays
Below are some examples of configuration displays:
[ EPC1 ] = (INLET) (SS) EPC #1 is used for an inlet of type split/splitless. It is not available for other uses.
26
Advanced User Guide
Configuration
[ EPC3 ] = (DET-EPC) (FID) gases to an FID.
EPC #3 is controlling detector
[ EPC6 ] = (AUX_EPC) (PCM) EPC #6 is controlling a two- channel pressure control module. FINLET (OK) 68 watts 21.7 This heater is connected to the front inlet. Status = OK, meaning that it is ready for use. At the time that the GC was turned on, the heater was drawing 68 watts and the inlet temperature was 21.7 C. [ F-DET ] = (SIGNAL) (FID) detector is type FID.
The signal board for the front
AUX 2 1 watts (No sensor) The AUX 2 heater is either not installed or not OK.
Unconfigured:
Accessory devices requiring GC power or communication must be assigned these GC resources before they can be used. To make this hardware element usable, first Unlock the GC Configuration on page 26 then go to the Unconfigured parameter and press [Mode/Type] to install it. If the hardware element you are configuring requires selection of additional parameters, the GC asks for that selection. If no parameters are required, press [Enter] at the GC prompt to install that element. You are required to power the GC off and then power the GC on to complete this configuration. After restarting the GC, a message reminding you of this change and its effect on the default method is displayed. If needed, change your methods to accommodate the new hardware.
Advanced User Guide
27
Configuration
Oven
See Unconfigured: on page 27 and Ignore Ready = on page 26.
Maximum temperature Sets an upper limit to the oven temperature. Used to prevent accidental damage to columns. The range is 70 to 450 C. Equilibration time The time after the oven approaches its setpoint before the oven is declared Ready. The range is 0 to 999.99 minutes. Used to ensure that the oven contents have stabilized before starting another run. Cryo These setpoints control liquid carbon dioxide (CO2 or liquid nitrogen (N2) cooling of the oven.
The cryogenic valve lets you operate the oven below ambient temperature. Minimum attainable oven temperature depends on the type of valve installed. The GC senses the presence and type of cryogenic valve and disallows setpoints if no valve is installed. When cryogenic cooling is not needed or cryogenic coolant is not available, the cryogenic operation should be turned off. If this is not done, proper oven temperature control may not be possible, particularly at temperatures near ambient.
External oven mode Isothermal internal oven and programmed external oven used to calculate column flow. Slow oven cool down mode On reduces the oven fan speed during the cool down cycle.
To configure the oven

1 Press [Config][Oven]. 2 Scroll to Maximum temperature. Enter a value and press
[Enter].
3 Scroll to Equilibration time. Enter a value and press [Enter]. 4 Scroll to Cryo. Press [On/Yes] or [Off/No]. If On, enter the
setpoints described in To configure the oven for cryogenic cooling on page 29.
5 Scroll to External oven mode. Press [On/Yes] or [Off/No].
28
Advanced User Guide
Configuration
6 Scroll to Slow oven cool down mode. Press [On/Yes] to run
the oven fan at reduced speed during cool down, or [Off/No] to run it at normal speed.
To configure the oven for cryogenic cooling

All cryogenic setpoints are in the [Config] [Oven] parameter list.
Cryo
[ON] enables cryogenic cooling, [OFF] disables it.
Quick cryo cool This feature is separate from Cryo. Quick cryo cool makes the oven cool faster after a run than it would without assistance. This feature is useful when maximum sample throughput is necessary, however it does use more coolant. Quick cryo cool turns off soon after the oven reaches its setpoint and Cryo takes over, if needed. Ambient temp The temperature in the laboratory. This setpoint determines the temperature at which cryogenic cooling is enabled:
Ambient temp + 25C, for regular cryo operation Ambient temp + 45C, for Quick Cryo Cool.
Cryo timeout Cryo timeout occurs, and the oven shuts off, when a run does not start within a specified time (10 to 120 minutes) after the oven equilibrates. Turning cryo timeout off disables this feature. We recommend that it be turned on because cryo timeout conserves coolant at the end of a sequence or if automation fails. Cryo fault Shuts the oven down if it does not reach setpoint temperature after 16 minutes of continuous cryo operation. Note that this is the time to reach the setpoint, not the time to stabilize and become ready at the setpoint. For example, with a cool on- column inlet and cryo control in the oven track mode, it may take the oven 20 to 30 minutes to achieve readiness.
If the temperature goes below the minimum allowed temperature (90C for liquid nitrogen,70C for liquid CO2), the oven will shut down.
Advanced User Guide
29
Configuration
Front Inlet/Back Inlet

See Unconfigured: on page 27 and Ignore Ready = on page 26.
To configure the Gas type

The GC needs to know what carrier gas is being used.
1 Press [Config] [Front Inlet] or [Config] [Back Inlet]. 2 Scroll to Gas type and press [Mode/Type]. 3 Scroll to the gas you will use. Press [Enter].
This completes carrier gas configuration.
To configure the MMI, PTV or COC coolant

Press [Config] [Front Inlet] or [Config][Back Inlet]. If the inlet has not been configured previously, a list of available coolants is displayed. Scroll to the desired coolant and press [Enter]. If oven cooling is installed, your choices are restricted to the coolant used by the oven or None. If the Cryo type selection is anything other than None, several other parameters appear.
Cryo [On/Yes] enables cryogenic cooling of the inlet at the specified Use Cryo temperature setpoint, [Off/No] disables cooling. Use cryo temperature This setpoint determines the temperature at which cryogenic cooling is used continuously. The inlet uses cryogen to achieve the initial setpoint. If the initial setpoint is below the Use Cryo temperature, cryogen is used continuously to achieve and maintain the setpoint. Once the inlet temperature program starts, the cryogen will be turned off when the inlet exceeds the Use Cryo temperature. If the initial setpoint is above the Use Cryo temperature, cryogen is used to cool the inlet until it reaches the setpoint and then it is turned off. At the end of a run, the inlet waits until the oven comes ready before it uses cryogen.
If the inlet is to be cooled during a run, cryogen will be used to achieve the setpoint. This may have a negative impact on the chromatographic performance of the oven and cause distorted peaks.
30
Advanced User Guide
Configuration
Cryo timeout Use this setting to conserve cryogenic fluid. If selected, the instrument shuts down the inlet and cryogenic (subambient) cooling (if installed) when no run starts in the number of minutes specified. The setpoint range is 2 to 120 minutes (default 30 minutes). Turning cryo timeout off disables this feature. We recommend cryo timeout enabling to conserve coolant at the end of a sequence or if automation fails. A Post Sequence method could also be used. Cryo fault Shuts down the inlet temperature if it does not reach setpoint in 16 minutes of continuous cryo operation. Note that this is the time to reach the setpoint, not the time to stabilize and become ready at the setpoint.
Shutdown behavior
Both Cryo timeout and Cryo fault can cause cryo shutdown. If this happens, the inlet heater is turned off and the cryo valve closes. The GC beeps and displays a message. The inlet heater is monitored to avoid overheating. If the heater remains on at full power for more than 2 minutes, the heater is shut down. The GC beeps and displays a message. To recover from either condition, turn the GC off, then on, or enter a new setpoint.
Advanced User Guide
31
Configuration
Column #
Length The length, in meters, of a capillary column. Enter 0 for a packed column or if the length is not known. Diameter The inside diameter, in millimeters, of a capillary column. Enter 0 for a packed column. Film thickness The thickness, in millimeters, of the stationary phase for capillary columns. Inlet
Identifies the source of gas for the column.
Outlet Identifies the device into which the column effluent flows. Thermal zone Identifies the device that controls the temperature of the column.
To configure a single column

You define a capillary column by entering its length, diameter, and film thickness. You then enter the device controlling the pressure at the Inlet (end of the column), the device controlling the pressure at the column Outlet, and the Thermal zone that controls its temperature. With this information, the instrument can calculate the flow through the column. This has great advantages when using capillary columns because it becomes possible to: Enter split ratios directly and have the instrument calculate and set the appropriate flow rates. Enter flow rate or head pressure or average linear velocity. The instrument calculates the pressure needed to achieve the flow rate or velocity, sets that, and reports all three values. Perform splitless injections with no need to measure gas flows. Choose any column mode. If the column is not defined, your choices are limited and vary depending on the inlet.
32
Advanced User Guide
Configuration
Except for the simplest configurations, such as a column connected to a specific inlet and detector, we recommend that you begin by making a sketch of how the column will be connected.
1 Press [Config] [Col 1] or [Config][Col 2], or press [Config][Aux
Col #] and enter the number of the column to be configured.

2 Scroll to the Length line, type the column length, in
meters, followed by [Enter].

3 Scroll to Diameter, type the column inside diameter in
microns, followed by [Enter].

4 Scroll to Film thickness, type the film thickness in microns,
followed by [Enter]. The column is now defined. If you do not know the column dimensionsthey are usually supplied with the columnor if you do not wish to use the GC calculating features, enter 0 for either Length or Diameter. The column will be not defined.
5 Scroll to Inlet. Press [Mode/Type] to select a gas pressure
control device for this end of the column. Selections include the installed GC inlets, and installed Aux and PCM channels. Select the appropriate gas pressure control device and press [Enter].
6 Scroll to Outlet. Press [Mode/Type] to select a gas pressure
control device for this end of the column. Selections include the installed Aux and PCM channels, and detectors. When a detector is selected, the outlet end of the column is controlled at 0 psig for the FID, TCD, FPD, NPD, and uECD or vacuum for the MSD. Select the appropriate gas pressure control device and press [Enter].
7 Scroll to Thermal zone. Press [Mode/Type] to see the
available choices. In most cases this will be GC oven, but you may have an MSD transfer line heated by an auxiliary zone, valves in a separately- heated valve box or other configurations. Select the appropriate Thermal zone and press [Enter]. This completes configuration for a single capillary column.
Advanced User Guide
33
Configuration
Additional notes on column configuration

Packed columns should be configured as column not defined. To do this, enter 0 for either column length or column diameter. You should check configurations for all columns to verify that they specify the correct pressure control device at each end. The GC uses this information to determine the flow path of the carrier gas. Only configure columns that are in current use in your GCs carrier gas flow path. Unused columns configured with the same pressure control device as a column in the current flow path cause incorrect flow results. It is possible, and sometimes appropriate, to configure both installed columns to the same inlet. When splitters or unions exist in the carrier gas flow path, without a GCs pressure control device monitoring the common junction point, the individual column flows cannot be controlled directly by the GC. The GC can only control the inlet pressure of the upstream column whose inlet end is attached to a GCs pressure control device. A column flow calculator available from Agilent, and provided with Agilent capillary flow devices, is used for determining pressures and flows at this type of junction. Some pneumatic setpoints change with oven temperature because of changes in column resistance and in gas viscosity. This may confuse users who observe pneumatics setpoints changing when their oven temperature changes. However, the flow condition in the column remains as specified by the column mode (constant flow or pressure, ramped flow or pressure) and the initial setpoint values.
To configure multiple columns

To configure multiple columns, repeat the procedure above for each column. These are the available choices for Inlet, Outlet, and Thermal zone. Some will not appear on your GC if the specific hardware is not installed.
34
Advanced User Guide
Configuration
Table 1
Inlet Front inlet Back inlet
Choices for column configuration

Outlet Front detector Back detector MSD Aux detector Aux 1 through 9 PCM A, B, and C Aux PCM A, B, and C Front inlet Back inlet Other Thermal zone GC oven Auxiliary oven Aux thermal zone 1 Aux thermal zone 2
Aux# 1 through 9 PCM A, B, and C Aux PCM A, B, and C Unspecified
Inlets and outlets

The pressure control devices at the inlet and outlet ends of a column, or series of columns in a flow path, control its gas flow. The pressure control device is physically attached to the column through a connection to a GC inlet, a valve, a splitter, a union, or other device. Table 2 Column inlet end
Choose:
If the column gas flow source is:
An inlet (SS, PP, COC, MMI, PTV, VI, or other) with electronic The inlet. pressure control A valve, such as gas sampling The auxiliary (Aux PCM) or pneumatics (PCM) control module channel that provides gas flow during the inject cycle. The Aux PCM or EPC channel that provides the makeup gas Unknown
A splitter with an EPC makeup gas supply A device with a manual pressure controller
Similar considerations apply for the column outlet end. When a column exits to a splitter, select the GCs pressure control source attached to the same splitter.
Advanced User Guide
35
Configuration
Table 3
Column outlet end

Choose: The detector. The Aux PCM or EPC channel that provides makeup gas flow to the splitter. Unknown
If the column exhausts into A detector A splitter with a makeup gas supply A device with a manual pressure controller
36
Advanced User Guide
Configuration
A simple example
An analytical column is attached at its inlet end to a spit/splitless inlet located at the front of the GC and the column outlet is attached to an FID located at the front detector position. Table 4
Column
Analytical column
Inlet Outlet Front FID Thermal zone GC oven
Analytical column Front split/splitless
Since only a single column is configured, the GC determines that it controls the inlet pressure to the column by setting the front inlet pressure and the outlet pressure is always atmospheric. The GC can calculate a pressure for the front inlet that can exactly overcome the resistance to flow presented by this column at any point during a run.
Slightly more complex example

A precolumn is followed by a AUX 1 pressure controlled splitter and two analytical columns. This requires three column descriptions. Table 5
Column 1 - Precolumn
Precolumn split to two analytical columns

Inlet Front inlet Outlet AUX 1 Front detector Back detector Thermal zone GC oven GC oven GC oven
2 - Analytical column AUX 1 3 - Analytical column AUX 1
The GC can calculate the flow through the precolumn using the precolumns physical properties to calculate the columns resistance to flow, along with the front inlet pressure and the AUX 1 pressure. Your analytical method can set this flow directly for the precolumn. For the flow in the two parallel analytical columns 1 and 2, the GC can use the columns physical properties to calculate the split flow through each individual column, at a given AUX 1 pressure, with both columns exiting to atmospheric pressure. Your analytical method can only set the flow for the lowest numbered column in a split , analytical column 2. If you try to set the flow for column #3, it will be ignored and the flow for column #2 will be used.
Advanced User Guide
37
Configuration
If other columns are currently defined, they may not use AUX 1, Front inlet, Front detector, or Back detector in their configuration.
Complicated example
The inlet feeds the analytical column which ends at a three- way splitter. The splitter has the column effluent and makeup gas coming in, and transfer lines (non- coated columns) to three different detectors. This is a case where a sketch is necessary.
Split/splitless inlet
Aux EPC
ECD
FPD
MSD
0.507 m x 0.10 mm x 0 m
0.532 m x 0.18 mm x 0 m
1.444 m x 0.18 mm x 0 m
30 m x 0.25 mm x 0.25 m HP-MS5
Table 6
Column
Splitter with makeup and multiple detectors

Inlet Front inlet Aux PCM 1 Aux PCM 1 Aux PCM 1 Outlet Aux PCM 1 MSD Front detector Back detector Thermal zone GC oven GC oven GC oven GC oven
1 - 30 m 0.25 mm 0.25 m 2 - 1.444 m 0.18 mm 0 m 3 - 0.507 m 0.10 mm 0 m 4 - 0.532 m 0.18 mm 0 m
The oven was chosen for the MSD line since most of it is in the oven. As in the previous examples, your analytical method can control the flow of column # 1 which has a GC pressure controlled inlet and outlet.
38
Advanced User Guide
Configuration
The flows to the three detectors are based on the pressure drops through the capillaries and their resistance to flow. An Agilent flow calculator provided with the capillary flow splitter device is used to size the length and diameter of these capillary sections to obtain the desired split ratios. Your analytical method can set the flow or pressure for column # 2, the lowest numbered column in the split. Use the value obtained from the Agilent flow calculator for this setpoint in your method.
Advanced User Guide
39
Configuration
Cryo Trap
This discussion assumes that the trap is mounted in position B, that you use liquid nitrogen coolant and control the trap with Thermal Aux 1. Configuration is in several parts: Configure the trap to the GC Configure a heater to the cryo trap. Configure the coolant. Configure the user- configurable heater. Reboot the GC.
Configure the cryo trap to the GC

1 Press [Config], then [Aux Temp #] and select Thermal Aux 1.
Press [Enter].
2 Press [Mode/Type]. Scroll to Install BINLET with BV Cryo and
press [Enter].
3 Press [Options], select Communications, and press [Enter].
Select Reboot GC and press [On/Yes] twice. This informs the GC that a cryo trap is installed at position B.
Configure a heater to the cryo trap

1 Press [Config], then [Aux Temp #], select Thermal Aux 1 and
press [Enter]. Select Auxiliary Type: Unknown and press [Mode/Type]. Select User Configurable Heater and press [Enter].
2 Press [Options], select Communications, and press [Enter].
Select Reboot GC and press [On/Yes] twice. This informs the GC that the heater parameters will be supplied by the user.
Configure the coolant

The GC can handle only one type of coolant. If the coolant has already been specified for some other device, then that same coolant must be specified here.
1 Press [Config], then [Aux Temp #]. 2 Select Thermal Aux 1 and press [Enter].
40
Advanced User Guide
Configuration
3 Scroll to Cryo Type (Valve BV).
If the value is not N2, press [Mode/Type], select N2 Cryo, press [Enter] and then [Clear]. This tells the GC what coolant will be used.
Configure the user-configurable heater

Many of the following steps tell you to reboot the GC. Ignore these requests by pressing [Clear]. Do not reboot until specifically told to do so in these instructions.
1 Press [Config] and select Aux 1. Press [Enter]. 2 Enter the following control values. Press [Enter], then
[Clear] after each one.

a Proportional Gain5.30 b Integral Time10 c Derivative Time1.00 d Mass (Watt- sec/deg)18 e Power (Watts)To find the watts to set here, scroll to
Back Inlet Status (BINLET). Note the watts value and enter it for this parameter.
f
Cryo Control ModePress [Mode/Type]. The first line should already be PTV. Select Cryo Trap.
g Zone Control modePress [Mode/Type] and select PTV. h SensorPress [Mode/Type] and select Thermocouple. i j
Maximum Setpoint400 Maximum Programming Rate720
Reboot the GC
Press [Options], select Communications, and press [Enter]. Select Reboot GC and press [On/Yes] twice.
Advanced User Guide
41
Configuration
Front Detector/Back Detector/Aux Detector/Aux Detector 2

See Ignore Ready = and Unconfigured: on page 27.
To configure the makeup/reference gas

The makeup gas line of your detector parameter list changes depending on your instrument configuration. If you have an inlet with the column not defined, the makeup flow is constant. If you are operating with column defined, you have a choice of two makeup gas modes. See About Makeup Gas on page 308 for details.
1 Press [Config][device], where [device] is one of the
following: [Front Det] [Back Det] [Aux detector 1] [Aux detector 2]

2 Scroll to Makeup gas type (or Makeup/reference gas type) and
press [Mode/Type].
3 Scroll to the correct gas and press [Enter].
Lit offset
The GC monitors the difference between the detector output with the flame lit and the output when the flame is not lit. If this difference falls below the setpoint, the GC assumes that the flame has gone out and tries to reignite it. See FID automatic reignition (Lit offset) on page 311 for details.
To configure the FPD heaters

The flame photometric detector (FPD) uses two heaters, one in the base and one near the combustion chamber. When configuring the FPD heaters, select Install Detector 2 htr rather than the default Install Detector (FPD).
42
Advanced User Guide
Configuration
Analog out 1/Analog out 2

Fast peaks
The GC allows you to output analog data at two speeds. The faster speedto be used only with the FID, FPD, and NPDallows minimum peak widths of 0.004 minutes (8 Hz bandwidth), while the standard speedwhich can be used with all detectors allows minimum peak widths of 0.01 minutes (3.0 Hz bandwidth). To use fast peaks:
1 Press [Config][Analog out 1] or [Config][Analog out 2]. 2 Scroll to Fast peaks and press [On/Yes].
The fast peaks feature does not apply to digital output. If you are using the fast peaks feature, your integrator must be fast enough to process data coming from the GC. Integrator bandwidth should be at least 15 Hz.
Advanced User Guide
43
Configuration
Valve Box
See Unconfigured: on page 27 and Ignore Ready = on page 26. The valve box mounts on top of the column oven. It may contain up to four valves mounted on heated blocks. Each block can accommodate two valves. Valve positions on the blocks are numbered. We suggest that valves be installed in the blocks in numeric order. All heated valves in a valve box are controlled by the same temperature setpoint.
To assign a GC power source to a valve box heater

1 Unlock the GC configuration, press the [Options] key, select
Keyboard & Display and press the [Enter] key. Scroll down to Hard Configuration Lock and press the [off] button.
2 Press [Config], scroll to Valve Box and press [Enter]. 3 With Unconfigured selected, press [Mode/type], select one of
the following and press [Enter]. Install heater A1 - for a valve box containing a single heater plugged into the connector labeled A1 on the valve box bracket. Install Heater A2 - for a valve box containing a single heater plugged into the connector labeled A2 on the valve box bracket. Install 2 htr A1 & A2 - for a valve box containing two heaters plugged into the connectors labeled AI and A2 on the valve box bracket. The valve box bracket is located inside the GC right side electrical compartment in the upper right location.
4 When prompted by the GC, turn the power off then on
again. This completes the configuration of the valve box. To set the valve box temperature for your method press the [valve #] key, and scroll to Valve Box.
44
Advanced User Guide
Configuration
Thermal Aux
See Unconfigured: on page 27 and Ignore Ready = on page 26. The auxiliary thermal controllers provide up to three channels of temperature control. These controllers are labeled Thermal Aux 1, Thermal Aux 2, and Thermal Aux 3.
To assign a GC power source to an Aux thermal zone

This procedure assigns a the heater power source from heater plug A1 or A2 to Thermal Aux 1, Thermal Aux 2, or Thermal Aux 3 temperature control zones.
1 Unlock the GC configuration, press [Options], select
2 Press [Config][Aux Temp #] and scroll to Thermal Aux 1,
Thermal Aux 2, or Thermal Aux 3 and press [Enter].

3 With Unconfigured selected, press [Mode/Type], and select:
Install Heater A1 if the heated device is plugged into the valve box bracket plug labeled A1. Install Heater A2 if the heated device is plugged into the valve box bracket plug labeled A2.
4 Press [Enter] after making selection. 5 When prompted by the GC, turn the power off then on
again.
To configure an MSD transfer line heater

1 Check that a power source for the MSD heater was
assigned. See To assign a GC power source to an Aux thermal zone on page 45.
Thermal Aux 2, or Thermal Aux 3 depending on where the MSD heater was assigned, and press [Enter].
3 Scroll to Auxiliary type, press [Mode/Type], scroll to and
select the MSD transfer line, and press [Enter].
Advanced User Guide
45
Configuration
To configure a nickel catalyst heater

1 Check that a power source for the Nickel Catalyst heater
was assigned. See To assign a GC power source to an Aux thermal zone on page 45.
Thermal Aux 2, or Thermal Aux 3 depending on where the Nickel Catalyst heater was assigned, and press [Enter].
select Nickel catalyst, and press [Enter].
To configure an AED transfer line heater

1 Check that a power source for the AED transfer line
heater was assigned. See To assign a GC power source to an Aux thermal zone on page 45.
Thermal Aux 2, or Thermal Aux 3 depending on where the AED transfer line heater was assigned, and press [Enter].
select the AED transfer line, and press [Enter].
46
Advanced User Guide
Configuration
PCM A/PCM B/PCM C

See Unconfigured: on page 27 and Ignore Ready = on page 26. A pressure control module (PCM) provides two channels of gas control. Channel 1 is a simple forward- pressure regulator that maintains a constant pressure at its output. With a fixed downstream restrictor, it provides constant flow. Channel 2 is more versatile. With the normal flow direction (in at the threaded connector, out via the coiled tubing), it is similar to channel 1. However with the flow direction reversed (some extra fittings will be needed), it becomes a backpressure regulator that maintains a constant pressure at its inlet. Thus channel 2 (reversed) behaves as a controlled leak. If the inlet pressure drops below setpoint, the regulator closes down. If inlet pressure rises above setpoint, the regulator bleeds off gas until the pressure returns to setpoint.
To assign a GC communication source to a PCM

2 Press [Config][Aux EPC #], scroll to a PCMx and press
[Enter].
3 With Unconfigured selected, press [Mode/Type], select Install
EPCx and press [Enter].

again. To configure the other parameters on this PCM, see To configure a PCM.
To configure a PCM
1 Press [Config][Aux EPC #], scroll to the PCMx and press
[Enter].
2 Scroll to Gas type, press [Mode/Type], make a selection and
press [Enter].
Advanced User Guide
47
Configuration
This completes configuration for Channel 1. The rest of the entries refer to Channel 2.
3 Scroll to Aux gas type, press [Mode/Type], make a selection
and press [Enter].

4 Scroll to Aux Mode:, press [Mode/Type], select one of the
following and press [Enter]: Forward Pressure Control - Aux channel Back Pressure Control- Aux channel For a definition of these terms see Pressure Control Modules on page 162. The pressure control mode for the main channel is set by pressing [Aux EPC #]. Select Mode: , press [Mode/Type], select the mode and press [Enter].
48
Advanced User Guide
Configuration
Pressure aux 1,2,3/Pressure aux 4,5,6/Pressure aux 7,8,9

See Ignore Ready = and Unconfigured: on page 27. An auxiliary pressure controller provides three channels of forward- pressure regulation. Three modules can be installed for a total of nine channels. The numbering of the channels depends on where the controller is installed. See Auxiliary Pressure Controllers on page 165 for details. Within a single module, channels are numbered from left to right (as seen from the back of the GC) and are labeled on the AUX EPC module.
To assign a GC communication source to an Aux EPC

2 Press [Config][Aux EPC #], select Aux EPC 1,2,3 or Aux EPC 4,5,6
or Aux EPC 7,8,9 and press [Enter].

3 With Unconfigured selected, press [Mode/Type], select Install
EPCx and press [Enter].

again. To configure the other parameters on this EPC, see To configure an auxiliary pressure channel.
To configure an auxiliary pressure channel

1 Press [Config][Aux EPC #], select Aux EPC 1,2,3 or Aux EPC 4,5,6
or Aux EPC 7,8,9 and press [Enter].

2 Select Chan x Gas type, press [Mode/Type], select the gas that
is plumbed to the channel and press [Enter].

3 If necessary, repeat the above step for the other two
channels on this EPC module.
Advanced User Guide
49
Configuration
Status
The [Status] key has two tables associated with it. You switch between them by pressing the key.
The Ready/Not Ready status table

This table lists parameters that are Not Ready or gives you a Ready for Injection display. If there are any faults, warnings, or method mismatches present, they are displayed here.
The setpoint status table

This table lists setpoints compiled from the active parameter lists on the instrument. This is a quick way to view active setpoints during a run without having to open multiple lists.
To configure the setpoint status table

You can change the order of the list. You might want the three most important setpoints to appear in the window when you open the table.
1 Press [Config] [Status]. 2 Scroll to the setpoint that should appear first and press
[Enter]. This setpoint will now appear at the top of the list.
3 Scroll to the setpoint that should appear second and
press [Enter]. This setpoint will now be the second item on the list.
4 And so on, until the list is in the order you wish.
50
Advanced User Guide
Configuration
Time
Press [Time] to open this function. The first line always displays the current date and time, and the last line always displays a stopwatch. The two middle lines vary:
Between runs During a run run.
Show last and next (calculated) run times. Show time elapsed and time remaining in the
During Post Run time.
Show last run time and remaining Post Run
To set time and date

1 Press [Config][Time]. 2 Select Time zone (hhmm) and enter the local time offset
from GMT using a 24 hour format.

3 Select Time (hhmm) and enter the local time. 4 Select Date (ddmmyy) and enter the date.
To use the stopwatch

1 Press [Time]. 2 Scroll to the time= line. 3 To begin the timed period press [Enter]. 4 To stop the timed period press [Enter]. 5 Press [Clear] to reset the stopwatch.
Advanced User Guide
51
Configuration
Valve #
Up to 4 valves can be mounted in a temperature- controlled valve box and are normally wired to the valve box bracket V1 through V4 plugs, located inside the electrical compartment. Additional valves or other devices (4 through 8) can be wired using the plug labeled EVENT on the back of the GC.
To configure a valve
1 Press [Config][Valve #] and enter the number (1 to 8) of
the valve you are configuring. The current valve type is displayed.
2 To change the valve type, press [Mode/Type], select the
new valve type, and press [Enter].
Valve types
Sampling Two- position (load and inject) valve. In load position, an external sample stream flows through an attached (gas sampling) or internal (liquid sampling) loop and out to waste. In inject position, the filled sampling loop is inserted into the carrier gas stream. When the valve switches from Load to Inject, a run starts if one is not already in progress. See the example in Gas sampling valve on page 358. Switching Two- position valve with four, six, or more ports. These are general- purpose valves used for such tasks as column selection, column isolation, and many others. For an example of valve control, see Simple valve: column selection on page 357. Multiposition Also called a stream selection valve. It selects one from a number of gas streams and feeds it to a sampling valve. The actuator may be ratchet- (advances the valve one position each time it is activated) or motor- driven. An example that combines a stream selection valve with a gas sampling valve is on page 359. Remote start Available selection when configuring valve #7 or #8 only. Use this selection when wires controlling an external device are attached to an internal pair of contacts controlled by the GC. Other Something else. Self- explanatory. Not installed
52
Advanced User Guide
Configuration
Front injector/Back injector

The GC supports two models of samplers. For the 7693A samplers, the GC recognizes which injector is plugged into which connector, INJ1 or INJ2. No configuration is needed. To move an injector from one inlet to another requires no settings: the GC detects the injector position. To configure the 7693A sampler system, see the 7693A Installation, Operation, and Maintenance manual. For the 7683 series samplers, normally the front inlets injector is plugged into the connection on the rear of the GC labeled INJ1. The rear inlets injector is plugged into the connection on the rear of the GC labeled INJ2. When a GC shares a single 7683 injector between two inlets, the injector is moved from one inlet to the other and the injectors plug- in on the rear of the GC is switched. To move the 7683 injector from one inlet on the GC to another without changing the injectors plug- in, use the Front/Back tower parameter.
Solvent Wash Mode (7683 ALS)

This section applies to the 7683 ALS system. To configure the 7693A sampler system, see the 7693A Installation, Operation, and Maintenance manual. Depending upon the installed injector and turret, these parameters may be available to configure multiple solvent wash bottles usage. If necessary, refer to your injector user documentation for details. A, BUse solvent bottle A if injector uses solvent A washes and solvent bottle B if injector uses solvent B washes. A-A2, B-B2Use solvent bottles A and A2 if injector uses solvent A washes and solvent bottles B and B2 if injector uses solvent B washes. The injector alternates between both bottles. A-A3, B-B3Use solvent bottles A, A2, and A3 if injector uses solvent A washes and solvent bottles B, B2, and B3 if injector uses solvent B washes. The injector alternates between all bottles.
Advanced User Guide
53
Configuration
To configure an injector (7683 ALS)

This section applies to the 7683 ALS system. To configure the 7693A sampler system, see the 7693A Installation, Operation, and Maintenance manual.
1 Press [Config][Front Injector] or [Config][Back Injector]. 2 Scroll to Front/Back tower. 3 Press [Off/No] to change the present tower position from
INJ1 to INJ2 or from INJ2 to INJ1.

4 If the installed turret has locations for multiple solvent
bottles, scroll to Wash Mode, press [Mode/Type], and then select 1, 2, or 3 bottles for each solvent and press [Enter].
5 Scroll to [Syringe size]. Enter the size of the syringe that is
installed and press [Enter].
54
Advanced User Guide
Configuration
Sample tray (7683 ALS)

This section applies to the 7683 ALS system. To configure the 7693A sampler system, see the 7693A Installation, Operation, and Maintenance manual.
1 Press [Config][Sample Tray]. 2 If the vial gripper is touching vials either too high or too
low for reliable pickup, scroll to Grip offset and press [Mode/Type] to select: Up to increase the gripper arm pickup height Default Down to decrease the gripper arm pickup height
3 Scroll to Bar Code Reader. 4 Press [On/Yes] or [Off/No] to control the following bar
code setpoints: Enable 3 of 9encodes both letters and numbers, plus a few punctuation marks, and message length can be varied to suit both the amount of data to be encoded and the space available Enable 2 of 5restricted to numbers but does allow variable message length Enable UPC coderestricted to numbers- only with fixed message length Enable checksumverifies that the checksum in the message matches the checksum calculated from the message characters, but does not include the checksum character in the returned message
5 Enter 3 as the BCR Position when the reader is installed in
the front of the tray. Positions 119 are available.
Advanced User Guide
55
Configuration
Instrument
1 Press [Config]. Scroll to Instrument and press [Enter]. 2 Scroll to Serial #. Enter a serial number and press [Enter].
This function can only be done by Agilent service personnel.

3 Scroll to Auto prep run. Press [On/Yes] to enable Auto prep
run, [Off/No] to disable it. See Pre Run and Prep Run on page 176 for details.
4 Scroll to Zero Init Data Files.
Press [On/Yes] to enable it. When it is On, the GC immediately begins to subtract the current detector output from all future values. This applies only to digital output, and is useful when a non- Agilent data system has problems with baseline data that is non- zero. Press [Off/No] to disable it. This is appropriate for all Agilent data systems.
5 Front inlet type: and Back inlet type: are both information
displays. The values are determined by the type of flow modules installed.
6 The Oven line displays the GC power configuration. 7 Press [Clear] to return to the Config menu or any other
function to end.
56
Advanced User Guide
3 Options
About Options 58 Calibration 59 Maintaining EPC calibrationinlets, detectors, PCM, and AUX 59 Auto zero septum purge 60 Auto flow zero 59 Zero conditions 60 Zero intervals 60 To zero a specific flow or pressure sensor 60 To zero all pressure sensors in all modules 61 Column calibration 61 Communication 65 Configuring the IP address for the GC 65 Keyboard and Display 66
57
Options
About Options
The [Options] key is used for a group of functions that are usually set on installation and seldom changed afterward. It accesses this menu:
Calibration Communication Keyboard and Display
58
Advanced User Guide
Options
Calibration
Press [Calibration] to list the parameters that can be calibrated. These include: Inlets Detectors ALS Columns Oven Atmospheric pressure In general, you will only need to calibrate the EPC modules and capillary columns. ALS, oven, and atmospheric pressure calibration should only be performed be trained service personnel. The calibration displays are discussed in the Agilent 7890A Service Manual.
Maintaining EPC calibrationinlets, detectors, PCM, and AUX

The EPC gas control modules contain flow and/or pressure sensors that are calibrated at the factory. Sensitivity (slope of the curve) is quite stable, but zero offset requires periodic updating.
Flow sensors
The split/splitless and purged packed inlet modules use flow sensors. If the Auto flow zero feature (see page 59) is on, they are zeroed automatically after each run. This is the recommended way. They can also be zeroed manuallysee To zero a specific flow or pressure sensor.
Pressure sensors
All EPC control modules use pressure sensors. They can be zeroed as a group or individually. There is no automatic zero for pressure sensors.
Auto flow zero

A useful calibration option is Auto flow zero. When it is On, after the end of a run the GC shuts down the flow of gases to an inlet, waits for the flow to drop to zero, measures and
Advanced User Guide
59
Options
stores the flow sensor output, and turns the gas back on. This takes about two seconds. The zero offset is used to correct future flow measurements. To activate this, select Calibration on the Options menu, then choose either Front inlet or Back inlet, press [Enter], and turn Auto flow zero on.
Auto zero septum purge

This is similar to Auto flow zero, but is for the septum purge flow.
Zero conditions
Flow sensors are zeroed with the carrier gas connected and flowing. Pressure sensors are zeroed with the supply gas line disconnected from the gas control module.
Zero intervals
Table 7
Sensor type Flow Pressure
Flow and Pressure Sensor Zero Intervals

Module type All Inlets Packed columns Small capillary columns (id 0.32 mm or less) Large capillary columns (id > 0.32 mm) Auxiliary channels Detector gases Every 12 months Every 12 months At 3 months, at 6 months, then every 12 months Every 12 months Every 12 months Zero interval Use Auto flow zero and/or Auto zero septum purge
To zero a specific flow or pressure sensor

1 Press [Options], scroll to Calibration, and press [Enter]. 2 Scroll to the module to be zeroed and press [Enter]. 3 Scroll to a zero line and press [Info]. The GC will remind
you of the conditions necessary for zeroing that specific sensor.
60
Advanced User Guide
Options
Flow sensors. Verify that the gas is connected and flowing (turned on). Pressure sensors. Disconnect the gas supply line at the back of the GC. Turning it off is not adequate; the valve may leak.
4 Press [On/Yes] to zero or [Clear] to cancel.
To zero all pressure sensors in all modules

1 Press [Service Mode], scroll to Diagnostics, and press [Enter]. 2 Scroll to Electronics and press [Enter]. 3 Scroll to Pneumatics and press [Enter]. 4 Scroll to Zero all pressure sensors and press [Info]. The GC
will remind you that all gas supplies must be disconnected at the back panel. Turning them off is not adequate; the valves may leak.
5 Press [On/Yes] to zero or [Clear] to cancel.
Column calibration
As you use a capillary column, you may occasionally trim off portions, changing the column length. If measuring the actual length is impractical, and if you are using EPC with a defined column, you can use an internal calibration routine to estimate the actual column length. Similarly, if you do not know the column internal diameter or believe it is inaccurate, you can estimate the diameter from related measurements. Before you can calibrate the column, make sure that: You are using a capillary column The column is defined There are no oven ramps The column gas source (usually the inlet) is On and non- zero Also note that column calibration fails if the calculated column length correction is > 5 m, or if the calculated diameter correction is > 20 m.
Calibration modes
There are three ways to calibrate the column length and/or diameter:
Advanced User Guide
61
Options
Calibrate using an actual measured column flow rate Calibrate using an unretained peak time (elution time) Calibrate both length and diameter using flow rate and elution time
CAUTION
When you measure the column flow rate, be sure to convert the measurement to normal temperature and pressure if your measurement device does not report data at NTP. If you enter uncorrected data, the calibration will be wrong. To estimate the actual column length or diameter from an elution time
1 Set oven ramp 1 to 0.00, then verify that the column is
defined.
2 Perform a run using an unretained compound and record
the elution time.

3 Press [Options], scroll to Calibration and press [Enter]. 4 From the calibration list, select the column and press
[Enter]. The GC displays the current calibration mode for the column.
5 To recalibrate or to change calibration mode, press
[Mode/Type] to see the column calibration mode menu.

6 Scroll to Length or Diameter and press [Enter]. The
following choices appear: Mode Measured flow Unretained peak Calculated length or Calculated diameter Not calibrated
7 Scroll to Unretained peak and enter the actual elution time
from the run performed above.

8 When you press [Enter], the GC will estimate the column
length or diameter based on the elution time input and will now use that data for all calculations.
62
Advanced User Guide
Options
To estimate the actual column length or diameter from the measured flow rate
defined.
2 Set the oven, inlet, and detectors temperatures to 35 C
and allow them to cool to room temperature.

3 Remove the column from the detector.
CAUTION
When you measure the column flow rate, be sure to convert the measurement to normal temperature and pressure if your measurement device does not report data at NTP. If you enter uncorrected data, the calibration will be wrong.
4 Measure the actual flow rate through the column using a
bubble meter. Record the value. Reinstall the column.


8 Scroll to Length or Diameter and press [Enter]. The
following choices appear: Mode Measured flow Unretained peak Calculated length or Calculated diameter Not calibrated
9 Scroll to Measured flow and enter the corrected column
flow rate (in mL min) from the run performed above.

To estimate the actual column length and diameter

defined.
2 Perform a run using an unretained compound and record
the elution time.
Advanced User Guide
63
Options
3 Set the oven, inlet, and detectors temperatures to 35 C
and allow them to cool to room temperature.

4 Remove the column from the detector.
CAUTION
When you measure the column flow rate, be sure to convert the measurement to normal temperature and pressure if your measurement device does not report data at NTP. If you enter uncorrected data, the calibration will be wrong.
5 Measure the actual flow rate through the column using a
bubble meter. Record the value. Reinstall the column.


9 Scroll to Length & diameter and press [Enter]. The following
choices appear: Mode Measured flow Unretained peak Calculated length Calculated diameter Not calibrated
10 Scroll to Measured flow and enter the corrected column
flow rate (in mL min) from the run performed above.

11 Scroll to Unretained peak and enter the actual elution time
from the run performed above.

64
Advanced User Guide
Options
Communication
Configuring the IP address for the GC
For network (LAN) operation, the GC needs an IP address. It can get this from a DHCP server, or it can be entered directly from the keyboard. In either case, see your LAN administrator.
To use a DHCP server

1 Press [Options]. Scroll to Communications and press [Enter]. 2 Scroll to Enable DHCP and press [On/Yes]. When prompted,
turn the GC off and then on again.
To set the LAN address at the keyboard

1 Press [Options]. Scroll to Communications and press [Enter]. 2 Scroll to Enable DHCP and, if necessary, press [Off/No].
Scroll to Reboot GC. Press [On/Yes] and [On/Yes].

3 Press [Options]. Scroll to Communications and press [Enter]. 4 Scroll to IP. Enter the numbers of the GC IP address,
separated by dots, and press [Enter]. A message tells you to power cycle the instrument. Do not power cycle yet. Press [Clear].
5 Scroll to GW. Enter the Gateway number and press [Enter].
A message tells you to power cycle the instrument. Do not power cycle yet. Press [Clear].
6 Scroll to SM and press [Mode/Type]. Scroll to the
appropriate subnet mask from the list given and press [Enter]. A message tells you to power cycle the instrument. Do not power cycle yet. Press [Clear].
7 Scroll to Reboot GC. Press [On/Yes] and [On/Yes] to power
cycle the instrument and apply the LAN setpoints.
Advanced User Guide
65
Options
Keyboard and Display

Press [Options] and scroll to Keyboard and Display. Press [Mode/Type]. The following parameters are turned on and off by pressing the [On/Yes] or [Off/No] keys.
Keyboard lock These keys and functions are operational when the keyboard lock is On:
[Start], [Stop], and [Prep Run] [Load][Method] and [Load][Seq] [Seq]to edit existing sequences [Seq Control]to start or stop sequences.
Hard configuration lock On prevents keyboard configuration changes; Off removes lock. Key click
Click sound when keys are pressed. Allows you to hear warning beeps.
Warning beep
Warning beep mode There are 9 different warning sounds that may be selected. This allows you to give multiple GCs individual voices. We suggest you experiment. Method modified beep Turn on for high pitched beep when method setpoint is modified.
Press [Mode/Type] to change the pressure units and radix type.
Pressure units
psipounds per square inch, lb/in2 barabsolute cgs unit of pressure, dyne/cm2 kPamks unit of pressure, 103 N/m2
Language Radix type 1,00
Select English or Chinese. Determines the numeric separator type1.00 or
66
Advanced User Guide
Options
Display saver If On, dims the display after a period of inactivity. If Off, disabled.
Advanced User Guide
67
Options
68
Advanced User Guide
4 Chromatographic Checkout
About Chromatographic Checkout 70 To Prepare for Chromatographic Checkout 71 To Check FID Performance 73 To Check TCD Performance 78 To Check NPD Performance 83 To Check uECD Performance 88 To Check FPD Performance (Sample 5188-5953) 93 To Verify FPD Performance (Sample 5188-5245) 101
69
About Chromatographic Checkout

The tests described in this section provide basic confirmation that the GC and detector can perform comparably to factory condition. However, as detectors and the other parts of the GC age, detector performance can change. The results presented here represent typical outputs for typical operating conditions and are not specifications. The tests assume the following: Use of an automatic liquid sampler. If not available, use a suitable manual syringe instead of the syringe listed. Use of a 10- L syringe in most cases. However, a 5- L syringe is an acceptable substitute for the 1- L injections described here. Use of the septa and other hardware (liners, jets, adapters, and so forth) described. If you substitute other hardware, performance can vary. Selected tests described in this section can be run automatically using the documentation and utility DVD provided with your GC.
70
Advanced User Guide
To Prepare for Chromatographic Checkout

Because of the differences in chromatographic performance associated with different consumables, Agilent strongly recommends using the parts listed here for all checkout tests. Agilent also recommends installing new consumable parts whenever the quality of the installed ones is not known. For example, installing a new liner and septum ensures that they will not contribute any contamination to the results.
1 Check the indicators/dates on any gas supply traps.
Replace/recondition expended traps.

2 Install new consumable parts for the inlet and prepare
the correct injector syringe (and needle, as needed). Table 8 Recommended parts for checkout by inlet type
Part number
Recommended part for checkout Split splitless inlet Syringe, 10-L O-ring Septum Liner
5181-1267 5188-5365 5183-4757 5183-4711 (FID) 5062-3587 or 5181-3316 (TCD, uECD, FPD, NPD)
Multimode inlet Syringe, 10-L O-ring Septum Liner Packed column inlet Syringe, 10-L O-ring Septum Cool on-column inlet Septum Septum nut Syringe, 5-L on-column 5183-4758 19245-80521 5182-0836 5181-1267 5080-8898 5183-4757 5181-1267 5188-6405 5183-4757 5188-6568
Advanced User Guide
71
Table 8
Recommended parts for checkout by inlet type (continued)

Part number 5182-0831 G4513-40529 G2913-60977 19245-20525
Recommended part for checkout 0.32-mm needle for 5-L syringe 7693A ALS: Needle support insert, COC 7683B ALS: Needle support assembly for 0.25/0.32 mm injections Insert, fused silica, 0.32-mm id PTV inlet Syringe, 10-Lfor septum head Syringe, 10-L, 23/42/HPfor septumless head Inlet adapter, Graphpak-2M Silver seal for Graphpak-2M Glass liner, multibaffle Teflon ferrule (septumless head) Microseal replacement (if installed) Ferrule, Graphpak-3D
5181-1267 5181-8809 5182-9761 5182-9763 5183-2037 5182-9748 5182-3444 5182-9749
72
Advanced User Guide
To Check FID Performance

1 Gather the following:
Evaluation column, HP- 5 30 m 0.32 mm 0.25 m (19091J- 413) FID performance evaluation (checkout) sample (5188- 5372) Chromatographic- grade isooctane 4- mL solvent and waste bottles or equivalent for autoinjector 2- mL sample vials or equivalent for sample
2 Verify the following:
Capillary column jet installed. If not, select and install a capillary column jet. Capillary column adapter installed (adaptable FID only). If not, install it. Chromatographic- grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air. Empty waste vials loaded in sample turret. 4- mL solvent vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Install the evaluation column. (See the procedure for the
SS, PP, COC, MMI, or PTV in the Maintenance manual.) Bake out the evaluation column for at least 30 min at 180 C. (See the procedure for the SS, PP, COC, MMI, or PTV in the Maintenance manual.) Be sure to configure the column.
4 Check the FID baseline output. The output should be
between 5 pA and 20 pA and relatively stable. (If using a gas generator or ultra pure gas, the signal may stabilize below 5 pA.) If the output is outside this range or unstable, resolve this problem before continuing.
5 If the output is too low:
Check that the electrometer is on. Check that the flame is lit (To light the FID flame on page 311).
6 Create or load a method with the parameter values listed
in Table 9.
Advanced User Guide
73
Table 9
FID Checkout Conditions
Column and sample Type Sample Column flow Column mode Split/splitless inlet Temperature Mode Purge flow Purge time Septum purge Gas saver Multimode inlet Mode Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Purge time Purge flow Septum purge Packed column inlet Temperature Septum purge Cool on-column inlet Temperature Septum purge PTV inlet Mode Splitless Oven Track 15 mL/min 250 C 3 mL/min Splitless 75 C 0.1 min 720 C/min 250 C 5.0 min 1.0 min 40 mL/min 3 mL/min 250 C Splitless 40 mL/min 0.5 min 3 mL/min Off HP-5, 30 m 0.32 mm 0.25 m (19091J-413) FID checkout 5188-5372 6.5 mL/min Constant flow
74
Advanced User Guide
Table 9
FID Checkout Conditions (continued)

75 C 0.1 min 720 C/min 350 C 2 min 100 C/min 250 C 0 min 0.5 min 40 mL/min 3 mL/min
Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Final time 2 Purge time Purge flow Septum purge Detector Temperature H2 flow Air flow Makeup flow (N2) Lit offset Oven Initial temp Initial time Rate 1 Final temp Final time ALS settings (if installed) Sample washes Sample pumps Sample wash volume Injection volume Syringe size Solvent A pre washes Solvent A post washes
300 C 30 mL/min 400 mL/min 25 mL/min Typically 2 pA
75 C 0.5 min 20 C/min 190 C 0 min
2 6 8 1 L 10 L 2 2
Advanced User Guide
75
Table 9
FID Checkout Conditions (continued)

8 0 0 0 Normal 0.20 0 6000 Fast, for all inlets except COC. 0 0
Solvent A wash volume Solvent B pre washes Solvent B post washes Solvent B wash volume Injection mode (7693A) Airgap Volume (7693A) Viscosity delay Inject Dispense Speed (7693A) Plunger speed (7683) PreInjection dwell PostInjection dwell Manual injection Injection volume Data system Data rate
1 L
5 Hz
7 If using a data system, prepare the data system to
perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram. If not using a data system, create a one sample sequence using the GC keypad.
8 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC. If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless
injection.
b When the GC becomes ready, inject 1 L of the
checkout sample and press [Start] on the GC.

9 The following chromatogram shows typical results for a
new detector with new consumable parts installed and nitrogen makeup gas.
76
Advanced User Guide
FID1 A, (C:\FID.D) pA 400 350 300 250 200 150 100 50 0 0 1 2 3 4
C15
C16
C13
C14
min
Advanced User Guide
77
To Check TCD Performance

Evaluation column, HP- 5 30 m 0.32 mm 0.25 m (19091J- 413) FID/TCD performance evaluation (checkout) sample (18710- 60170) 4- mL solvent and waste bottles or equivalent for autoinjector Chromatographic- grade hexane 2- mL sample vials or equivalent for sample Chromatographic- grade helium as carrier, makeup, and reference gas
Chromatographic- grade gases plumbed and configured: helium as carrier gas and reference gas. Empty waste vials loaded in sample turret. 4- mL solvent vial with diffusion cap filled with hexane and inserted in Solvent A injector position.
SS, PP, COC, MMI, or PTV in the Maintenance manual.) Bake out the evaluation column for at least 30 min at 180 C. (See the procedure for the SS, PP, COC, MMI, or PTV in the Maintenance manual.) Configure the column
in Table 10. Table 10 TCD Checkout Conditions
Column and sample Type Sample Column flow Column mode Split/splitless inlet Temperature 250 C HP-5, 30 m 0.32 mm 0.25 m (19091J-413) FID/TCD checkout 18710-60170 6.5 mL/min Constant flow
78
Advanced User Guide
Table 10
Mode Purge flow Purge time Septum purge
TCD Checkout Conditions (continued)

Splitless 60 mL/min 0.75 min 3 mL/min
Multimode inlet Mode Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Purge time Purge flow Septum purge Packed column inlet Temperature Septum purge Cool on-column inlet Temperature Septum purge PTV inlet Mode Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Final time 2 Purge time Purge flow Splitless 40 C 0.1 min 720 C/min 350 C 2 min 100 C/min 250 C 0 min 0.5 min 40 mL/min Oven track 15 mL/min 250 C 3 mL/min Splitless 40 C 0.1 min 720 C/min 350 C 2 min 1.0 min 40 mL/min 3 mL/min
Advanced User Guide
79
Table 10
Septum purge Detector Temperature

3 mL/min
300 C 20 mL/min 2 mL/min < 30 display counts on Agilent ChemStation (< 750 V)
Reference flow (He) Makeup flow (He) Baseline output Oven Initial temp Initial time Rate 1 Final temp Final time Rate 2 Final temp Final time ALS settings (if installed) Sample washes Sample pumps Sample wash volume Injection volume Syringe size Solvent A pre washes Solvent A post washes Solvent A wash volume Solvent B pre washes Solvent B post washes Solvent B wash volume Injection mode (7693A) Airgap Volume (7693A) Viscosity delay Inject Dispense Speed (7693A)
40 C 0 min 20 C/min 90 C 0 min 15 C/min 170 C 0 min
2 6 8 1 L 10 L 2 2 8 0 0 0 Normal 0.20 0 6000
80
Advanced User Guide
Table 10

Fast, for all inlets except COC. 0 0
Plunger speed (7683) PreInjection dwell PostInjection dwell Manual injection Injection volume Data system Data rate
1 L
5 Hz
5 Display the signal output. A stable output at any value
between 12.5 and 750 V (inclusive) is acceptable. If the baseline output is < 0.5 display units (< 12.5 V), verify that the detector filament is on. If the offset is still < 0.5 display units (< 12.5 V), your detector requires service. If baseline output is > 30 display units (> 750 V), there may be chemical contamination contributing to the signal. Bakeout the TCD. If repeated cleanings do not give an acceptable signal, check gas purity. Use higher purity gases and/or install traps.
perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
7 Start the run.
injection.

new detector with new consumable parts installed.
Advanced User Guide
81
25 uV 70 C14 60 C15 C16
50
40
30
20 2 4 Time (min.) 6 8
82
Advanced User Guide
To Check NPD Performance

Evaluation column, HP- 5 30 m 0.32 mm 0.25 m (19091J- 413) NPD performance evaluation (checkout) sample (18789- 60060) 4- mL solvent and waste bottles or equivalent for autoinjector. Chromatographic- grade isooctane 2- mL sample vials or equivalent for sample.
Capillary column jet installed. If not, select and install a capillary column jet. Capillary column adapter installed. If not, install it. Chromatographic- grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air. Empty waste vials loaded in sample turret. 4- mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 If present, remove any protective caps from the inlet
manifold vents.
SS, PP, COC, MMI, or PTV in the Maintenance manual.) Bake out the evaluation column for at least 30 min at 180 C. (See the procedure for the SS, PP, COC, MMI, or PTV in the Maintenance manual.) Be sure to configure the column
in Table 11. Table 11 NPD Checkout Conditions
Column and sample Type Sample Column mode HP-5, 30 m 0.32 mm 0.25 m (19091J-413) NPD checkout 18789-60060 Constant flow
Advanced User Guide
83
Table 11
Column flow
NPD Checkout Conditions (continued)

6.5 mL/min (helium)
Split/splitless inlet Temperature Mode Purge flow Purge time Septum purge Multimode inlet Mode Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Purge time Purge flow Septum purge Packed column inlet Temperature Septum purge Cool on-column inlet Temperature Septum purge PTV inlet Mode Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Splitless 60 C 0.1 min 720 C/min 350 C 2 min 100 C/min 250 C Oven track 15 mL/min 200 C 3 mL/min Splitless 60 C 0.1 min 720 C/min 350 C 2 min 1.0 min 60 mL/min 3 mL/min 200 C Splitless 60 mL/min 0.75 min 3 mL/min
84
Advanced User Guide
Table 11
Final time 2 Purge time Purge flow Septum purge Detector Temperature H2 flow Air flow

0 min 0.75 min 60 mL/min 3 mL/min
300 C 3 mL/min 60 mL/min Makeup + column = 10 mL/min 30 display units (30 pA)
Makeup flow (N2) Output Oven Initial temp Initial time Rate 1 Final temp Final time ALS settings (if installed) Sample washes Sample pumps Sample wash volume Injection volume Syringe size Solvent A pre washes Solvent A post washes Solvent A wash volume Solvent B pre washes Solvent B post washes Solvent B wash volume Injection mode (7693A) Airgap Volume (7693A) Viscosity delay
60 C 0 min 20 C/min 200 C 3 min
2 6 8 1 L 10 L 2 2 8 0 0 0 Normal 0.20 0
Advanced User Guide
85
Table 11

6000 Fast, for all inlets except COC. 0 0
Inject Dispense Speed (7693A) Plunger speed (7683) PreInjection dwell PostInjection dwell Manual injection Injection volume Data system Data rate
1 L
5 Hz
7 Start the run.
If performing an injection using an autosampler, start the run using the data system, or creating a one sample sequence and pressing [Start] on the GC. If performing a manual injection (with or without a data system):
injection.

86
Advanced User Guide
NPD1 B, (C:\NPD.D) pA 70
Malathion
60
Azobenzene
50
40
30
20 Octadecane 10 1 2 3 4 5 6 7 8 9 m
Advanced User Guide
87
To Check uECD Performance

Evaluation column, HP- 5 30 m 0.32 mm 0.25 m (19091J- 413) uECD performance evaluation (checkout) sample (1871360040, Japan: 5183- 0379) 4- mL solvent and waste bottles or equivalent for autoinjector. Chromatographic- grade isooctane 2- mL sample vials or equivalent for sample.
Clean fused silica indented mixing liner installed. If not, install it. Chromatographic- grade gases plumbed and configured: helium for carrier gas, nitrogen for makeup. Empty waste vials loaded in sample turret. 4- mL vial with diffusion cap filled with hexane and inserted in Solvent A injector position.
SS, PP, COC, MMI, or PTV in the Maintenance manual.) Bake out the evaluation column for at least 30 minutes at 180 C. (See the procedure for the SS, PP, COC, MMI, or PTV in the Maintenance manual.) Be sure to configure the column.
4 Display the signal output to determine baseline output. A
stable baseline output at any value between 0.5 and 1000 Hz (ChemStation display units) (inclusive) is acceptable. If the baseline output is < 0.5 Hz, verify that the electrometer is on. If the offset is still < 0.5 Hz, your detector requires service. If the baseline output is > 1000 Hz, there may be chemical contamination contributing to the signal. Bakeout the uECD. If repeated cleanings do not give an acceptable signal, check gas purity. Use higher purity gases and/or install traps.
in Table 12.
88
Advanced User Guide
Table 12
uECD Checkout Conditions
Column and sample Type Sample Column mode Column flow Split/splitless inlet Temperature Mode Purge flow Purge time Septum purge Multimode inlet Mode Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Purge time Purge flow Septum purge Packed column inlet Temperature Septum purge Cool on-column inlet Temperature Septum purge PTV inlet Mode Splitless Oven track 15 mL/min 200 C 3 mL/min Splitless 80 C 0.1 min 720 C/min 250 C 5 min 1.0 min 60 mL/min 3 mL/min 200 C Splitless 60 mL/min 0.75 min 3 mL/min HP-5, 30 m 0.32 mm 0.25 m (19091J-413 ECD checkout (18713-60040 or Japan: 5183-0379) Constant flow 6.5 mL/min (helium)
Advanced User Guide
89
Table 12
uECD Checkout Conditions (continued)

Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Final time 2 Purge time Purge flow Septum purge Detector Temperature Makeup flow (N2) Baseline output Oven Initial temp Initial time Rate 1 Final temp Final time ALS settings (if installed) Sample washes Sample pumps Sample wash volume Injection volume Syringe size Solvent A pre washes Solvent A post washes Solvent A wash volume Solvent B pre washes
300 C 30 mL/min (constant + makeup) Should be < 1000 display counts in Agilent ChemStation (< 1000 Hz)
80 C 0 min 15 C/min 180 C 10 min
2 6 8 1 L 10 L 2 2 8 0
90
Advanced User Guide
Table 12
uECD Checkout Conditions (continued)

0 0 Normal 0.20 0 6000 Fast, for all inlets except COC. 0 0
Solvent B post washes Solvent B wash volume Injection mode (7693A) Airgap Volume (7693A) Viscosity delay Inject Dispense Speed (7693A) Plunger speed (7683) PreInjection dwell PostInjection dwell Manual injection Injection volume Data system Data rate
1 L
5 Hz
7 Start the run.
injection.

Advanced User Guide
91
ECD1 B, (C:\ECD.D) Hz 12000 Lindane (18713-60040 5183-0379)
10000
8000 Aldrin (18713-60040)
6000
4000
2000
0 2 4 6 8 10 12 min
92
Advanced User Guide
To Check FPD Performance (Sample 5188-5953)

To check FPD performance, first check the phosphorus performance, then the sulfur performance.
Preparation
Evaluation column, HP- 5 30 m 0.32 mm 0.25 m (19091J- 413) FPD performance evaluation (checkout) sample (5188- 5953) Phosphorus filter Sulfur filter and filter spacer 4- mL solvent and waste bottles or equivalent for autoinjector. 2- mL sample vials or equivalent for sample. Chromatographic- grade isooctane for syringe wash solvent.
Capillary column adapter installed. If not, install it. Chromatographic- grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air. Empty waste vials loaded in sample turret. 4- mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Verify that the Lit Offset is set appropriately. Typically, it
should be about 2.0 pA for the checkout method.

SS, PP, COC, MMI, or PTV in the Maintenance manual.) Set the oven, inlet, and detector to 250 C and bake out for at least 15 minutes. (See the procedure for the SS, PP, COC, MMI, or PTV in the Maintenance manual.) Be sure to configure the column.
Phosphorus performance
5 If it is not already installed, install the phosphorus filter. 6 Create or load a method with the parameter values listed
in Table 13.
Advanced User Guide
93
Table 13
FPD Checkout Conditions (P)
Column and sample Type Sample Column mode Column pressure Split/splitless inlet Temperature Mode Purge flow Purge time Septum purge Multimode inlet Mode Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Purge time Purge flow Septum purge Packed column inlet Temperature Septum purge Cool on-column inlet Temperature Septum purge PTV inlet Mode Inlet temperature Splitless 75 C Oven track 15 mL/min 200 C 3 mL/min Splitless 75 C 0.1 min 720 C/min 250 C 5.0 min 1.0 min 60 mL/min 3 mL/min 200 C Split/splitless Splitless 60 mL/min 0.75 min 3 mL/min HP-5, 30 m 0.32 mm 0.25 m (19091J-413) FPD checkout (5188-5953) Constant pressure 25 psi
94
Advanced User Guide
Table 13
Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Final time 2 Purge time Purge flow Septum purge Detector Temperature Hydrogen flow
FPD Checkout Conditions (continued)(P)

0.1 min 720 C/min 350 C 2 min 100 C/min 250 C 0 min 0.75 min 60 mL/min 3 mL/min
200 C (On) 75 mL/min (On) 100 mL/min (On) Constant makeup flow OFF 60 mL/min (On) Nitrogen On Typically 2 pA On
Air (Oxidizer) flow Mode Makeup flow Makeup gas type Flame Lit offset High voltage Oven Initial temp Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Final time 2 ALS settings (if installed) Sample washes
70 C 0 min 25 C/min 150 C 0 min 5 C/min 190 C 4 min
Advanced User Guide
95
Table 13
Sample pumps
FPD Checkout Conditions (continued)(P)

6 8 1 L 10 L 2 2 8 0 0 0 Normal 0.20 0 6000 Fast, for all inlets except COC. 0 0
Sample wash volume Injection volume Syringe size Solvent A pre washes Solvent A post washes Solvent A wash volume Solvent B pre washes Solvent B post washes Solvent B wash volume Injection mode (7693A) Airgap Volume (7693A) Viscosity delay Inject Dispense Speed (7693A) Plunger speed (7683) PreInjection dwell PostInjection dwell Manual injection Injection volume Data system Data rate
1 L
5 Hz
7 Ignite the FPD flame, if not lit. 8 Display the signal output and monitor. This output
typically runs between 40 and 55 but can be as high as 70. Wait for the output to level off. This takes approximately 1 hour. If the baseline output is too high: Check column installation. If installed high, the stationery phase burns out and increases measured output. Check for leaks. Bake out the detector and column at 250 C. Wrong flows set for installed filter.
96 Advanced User Guide
If the baseline output is zero, verify the electrometer is on and the flame is lit.
10 Start the run.
injection.

Methylparathion
Isooctane
Advanced User Guide
97
Table 14
FPD P filter MDL (pg/sec) Peak area Signal height Noise
Evaluating checkout runs

Typical range after 24 hours 0.06 to 0.08 19000 to 32000 5000 to 11000 1.6 to 3.0 0.05 to 0.07 34 to 80 Limits at installation 0.10 19000 4 80
Half-width (min) Output
Sulfur performance
12 Install the sulfur filter and filter spacer. 13 Make the following method parameter changes.
Table 15
Parameter H2 flow Air flow
Sulfur method parameters (S)

Value ( mL/min) 50 60
14 Ignite the FPD flame if not lit. 15 Display the signal output and monitor. This output
typically runs between 50 and 60 but can be as high as 70. Wait for the output to level off. This takes approximately 1 hour. If the baseline output is too high: Check column installation. If installed high, the stationery phase burns out and increases measured output. Check for leaks. Bake out the detector and column at 250 C. Wrong flows set for installed filter. If the baseline output is zero, verify the electrometer is on and the flame is lit.
98
Advanced User Guide
17 Start the run.
injection.

Tributyl phosphate
Isooctane
Table 16
FPD S filter MDL (pg/s) Peak area Signal height

Typical range after 24 hours 3.8 to 5 8000 to 19000 2500 to 6000 Limits at installation 6 8000
Advanced User Guide
99
Table 16
FPD S filter Noise

Typical range after 24 hours 2 to 4 0.06 to 0.08 34 to 65 Limits at installation 5 70
100
Advanced User Guide
To Verify FPD Performance (Sample 5188-5245)

To verify FPD performance, first check the phosphorus performance, then the sulfur performance.
Preparation
Evaluation column, DB5 15 m 0.32 mm 1.0 m (123- 5513) FPD performance evaluation (checkout) sample (5188- 5245) Phosphorus filter Sulfur filter and filter spacer 4- mL solvent and waste bottles or equivalent for autoinjector. 2- mL sample vials or equivalent for sample. Chromatographic- grade isooctane for syringe wash solvent.
Capillary column adapter installed. If not, install it. Chromatographic- grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air. Empty waste vials loaded in sample turret. 4- mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Verify the lit offset is set appropriately. Typically, it
should be about 2.0 pA for the checkout method.

SS, PP, COC, MMI, or PTV in the Maintenance manual.) Set the oven, inlet, and detector to 250 C and bake out for at least 15 minutes. (See the procedure for the SS, PP, COC, MMI, or PTV in the Maintenance manual.) Configure the column.
Phosphorus performance
5 If it is not already installed, install the phosphorus filter. 6 Create or load a method with the parameter values listed
in Table 17.
Advanced User Guide
101
Table 17
FPD Phosphorus Checkout Conditions
Column and sample Type Sample Column mode Column flow Split/splitless inlet Temperature Mode Total purge flow Purge flow Purge time Septum purge Multimode inlet Mode Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Purge time Purge flow Septum purge Packed column inlet Temperature Septum purge Cool on-column inlet Temperature Septum purge PTV inlet Mode Splitless Oven track 15 mL/min 250 C 3 mL/min Splitless 80 C 0.1 min 720 C/min 250 C 5.0 min 1.0 min 60 mL/min 3 mL/min 250 C Splitless 69.5 mL/min 60 mL/min 0.75 min 3 mL/min DB-5MS, 15 m 0.32 mm 1.0 m (123-5513) FPD checkout (5188-5245) Constant flow 7.5 mL/min
102
Advanced User Guide
Table 17
FPD Phosphorus Checkout Conditions (continued)

Inlet temperature Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Final time 2 Purge time Purge flow Septum purge Detector Temperature Hydrogen flow Air (oxidizer) flow Mode Makeup flow Makeup gas type Flame Lit offset High voltage Oven Initial temp Initial time Rate 1 Final temp Final time Rate 2 Final temp 2 Final time 2 ALS settings (if installed)
200 C (On) 75.0 mL/min (On) 100.0 mL/min (On) Constant makeup flow Off 60.0 mL/min (On) Nitrogen On Typically 2 pA On
70 C 0 min 10 C/min 105 C 0 min 20 C/min 190 C 7.25 min for sulfur 12.25 min for phosphorus
Advanced User Guide
103
Table 17
FPD Phosphorus Checkout Conditions (continued)

2 6 8 1 L 10 L 2 2 8 0 0 0 Normal 0.20 0 6000 Fast, for all inlets except COC. 0 0
Sample washes Sample pumps Sample wash volume Injection volume Syringe size Solvent A pre washes Solvent A post washes Solvent A wash volume Solvent B pre washes Solvent B post washes Solvent B wash volume Injection mode (7693A) Airgap Volume (7693A) Viscosity delay Inject Dispense Speed (7693A) Plunger speed (7683) PreInjection dwell PostInjection dwell Manual injection Injection volume Data System Data rate
1 L
5 Hz
typically runs between 40 and 55 but can be as high as 70. Wait for the output to level off. This takes approximately 1 hour. If the baseline output is too high: Check column installation. If installed high, the stationery phase burns out and increases measured output. Check for leaks. Bake out the detector and column at 250 C.
Wrong flows set for installed filter If the baseline output is zero, verify the electrometer is on and the flame is lit.
10 Start the run.
injection.

Tributylphosphate
Isooctane
t-Butyldisulfide
Advanced User Guide
105
Table 18
FPD P filter MDL (pg/sec) Peak area Signal height Noise

Typical range after 24 hours 0.06 to 0.08 19000 to 32000 5000 to 11000 1.6 to 3.0 0.05 to 0.07 34 to 80 Limits at installation 0.10 19000 4 80
Sulfur performance
12 Install the sulfur filter. 13 Make the following method parameter changes.
Table 19
Parameter H2 flow Air flow
Sulfur method parameters

Value ( mL/min) 50 60
typically runs between 50 and 60 but can be as high as 70. Wait for the output to level off. This takes approximately 2 hours. If the baseline output is too high: Check column installation. If installed high, the stationery phase burns out and increases measured output. Check for leaks. Bake out the detector and column at 250 C. Wrong flows set for installed filter If the baseline output is zero, verify the electrometer is on and the flame is lit.
106
Advanced User Guide
perform one run using the loaded checkout method. Make sure the data system will output a chromatogram.
17 Start the run.
injection.

t-Butyldisulfide
1-Dodecanethiol
Isooctane
Table 20
FPD S filter MDL (pg/s) Peak area Signal height

Typical range after 24 hours 3.8 to 5 8000 to 19000 2500 to 6000 Limits at installation 6 8000
Advanced User Guide
107
Table 20
FPD S filter Noise

Typical range after 24 hours 2 to 4 0.06 to 0.08 34 to 65 Limits at installation 5 70
108
Advanced User Guide
5 Methods and Sequences

Creating Methods 110 To program a method 111 To program the ALS 111 To program the ALS sampler tray 111 To program the 7683B ALS bar code reader 112 To save a method 113 To load a stored method 113 Method mismatch 114 Creating Sequences 115 About the priority sequence 115 To program a sequence 116 To program a priority sequence 116 To program an ALS subsequence 117 To program a valve subsequence 117 To program post sequence events 117 To save a sequence 118 To load a stored sequence 118 To determine sequence status 118 To start a sequence 118 To pause and resume a sequence 119 To stop a sequence 119 To abort a sequence 119
109
Creating Methods
A method is the group of setpoints needed to run a single sample on the GC, such as oven temperature programs, pressure programs, inlet temperatures, sampler parameters, etc. A method is created by saving a group of setpoints as a numbered method using the [Store] key. At least 10 methods can be stored. Components for which setpoint parameters can be stored are shown in Table 21. Table 21
Component Oven Valve 18 Front and back inlet Columns 1 to 6 Front and back detector Analog 1 and 2 Front and back injector (see Table 22)
Setpoint parameter components

Component Aux temp Aux EPC Aux column Aux detector 1 and 2 Post run Run table Sample tray
Table 22 lists the setpoint parameters for the 7683B ALS. Table 22
Parameter Injection volume Viscosity delay Inject Dispense Speed Sample pumps Sample washes Solvent A post washes Solvent A pre washes Solvent B post washes Solvent B pre washes Solvent B wash volume
7683B ALS setpoint parameters

Parameter Sample Draw Speed Sample Disp Speed Solvent Draw Speed Solvent Disp Speed Slow plunger Pre dwell time Post dwell time Sample offset Injection Reps Injection Delay
110
Advanced User Guide
The GC also saves ALS setpoints. See the 7693A Installation, Operation, and Maintenance manual for details on its setpoints. Setpoint parameters are saved when the GC is turned off and loaded when you turn the instrument back on. However, if the hardware was changed while the instrument was turned off, it may not be possible to restore all setpoints in the method.
To program a method
1 Individually select each component for which setpoint
parameters are appropriate for your method. (See Table 21.)

2 Examine the current setpoints and modify as desired.
Repeat for each component as appropriate.

3 Examine the current setpoints for the ALS, if appropriate,
and modify as desired. (See To program the ALS on page 111.)

4 Save the setpoints as a stored method. (See To save a
method on page 113.)
To program the ALS

1 Press [Front Injector] or [Back Injector]. 2 Scroll to the desired setpoint. (See Table 22.) 3 Enter a setpoint value. 4 Examine the current setpoints for the sampler tray, if
appropriate, and modify as desired. (See To program the ALS sampler tray on page 111.)
5 Examine the current setpoints for the bar code reader, if
appropriate, and modify as desired. (See To program the 7683B ALS bar code reader on page 112.)
6 Save the setpoints as a stored method. (See To save a
method on page 113.)
To program the ALS sampler tray

For the 7693A sampler tray, see the 7693A Installation, Operation, and Maintenance manual.
Advanced User Guide
111
For the 7683B sampler tray:

1 Press [Sample tray]. 2 Press [On/Yes] to enable the barcode reader (if present) or
[Off/No] to disable it.
Configuration issues
1 To edit the sample tray configuration setpoints, press
[Config][Sample Tray]. Normally, no tray configuration is required. If using a bar code reader and the tray gripper arm has difficulties retrieving a vial from the bar code reader, adjust the gripper offset (step 2). If the sample vial contacts the side of the turret hole when the tray delivers or retrieves the sample vial, then adjust the injector offset (step 3).
2 Scroll to Grip offset and press [Mode/Type]. Select from:
Up to raise the gripper arm pickup height Default Down to lower the gripper arm pickup height and press [Enter].
3 Scroll to Front Injector Offset or Back Injector Offset and press
[Mode/Type]. Select from: Clockwise to have the gripper arm meet the turret at a further clockwise position (relative to turret rotation) Default CounterClockwise to have the gripper arm meet the turret at a further counterclockwise position (relative to turret rotation) and press [Enter].
To program the 7683B ALS bar code reader

For the 7693A sampler bar code reader, see the 7693A Installation, Operation, and Maintenance manual.
1 Press [Sample tray]. 2 Scroll to Enable bar code reader and press [On/Yes] to enable
or [Off/No] to disable the bar code reader.
112
Advanced User Guide
Configuration issues
1 To edit the bar code configuration setpoints, press
[Config][Sample Tray].
2 Select Bar Code Reader. 3 Press [On/Yes] or [Off/No] to control the following bar
code setpoints: Enable 3 of 9encodes both letters and numbers, plus a few punctuation marks, and message length can be varied to suit both the amount of data to be encoded and the space available Enable 2 of 5restricted to numbers but does allow variable message length Enable UPC coderestricted to numbers- only with fixed message length Enable checksumverifies that the checksum in the message matches the checksum calculated from the message characters, but does not include the checksum character in the returned message
4 Enter 3 as the BCR Position when the reader is installed in
the front of the tray. Positions 119 are available.
To save a method
1 Press [Method] and scroll to the desired method number. 2 Press [Store] and [On/Yes] to store the new method using
the chosen number. Alternatively, press [Off/No] to return to the stored methods list without saving the method. A message is displayed if a method with the number you selected already exists. Press [On/Yes] to replace the existing method or [Off/No] to return to the stored methods list without saving the method.
To load a stored method

Press [Load][Method]. Supply the method number and press [Enter]. The specified method will replace the current active method.
Advanced User Guide
113
Method mismatch
This section applies only to a standalone (not connected to a data system) GC. When a data system, such as a ChemStation or EZChrom Elite, controls the GC, methods are stored in the data system and can be edited there. See your data system documentation for more information. Suppose your standalone GC is equipped with a single FID. You have created and saved methods that use this detector. Now you remove the FID and install a TCD in its place. When you try to load one of your stored methods, you observe an error message saying that the method and the hardware do not match. The problem is that the actual hardware is no longer the same as the hardware configuration saved in the method. The method cannot run because it does not know how to operate the recently- added TCD. On inspecting the method, you find that the detector- related parameters have all been reset to the default values.
Correcting a method mismatch on a standalone GC

This problem can be avoided if you follow this procedure for any hardware change, even including the simple replacement of a defective detector board.
1 Before changing any hardware, press [Config][hardware
module], where [hardware module] is the device you intend to replace.

2 Press [Mode/Type]. Select Remove module and press [Enter].
The module is now Unconfigured.

3 Turn the GC off. 4 Make the hardware change that you intended (in this
example, remove the FID and its flow module and replace them with the TCD and its module).
5 Turn the GC on. Press [Config][hardware module]. 6 Press [Mode/Type]. Select Install module and press [Enter].
The GC will install the new hardware module, which corrects the active method (but not the stored one!).
7 Save the corrected method using the same number (which
overwrites the stored method) or a new number (which saves both versions of the method).
114
Advanced User Guide
Creating Sequences
A sequence specifies the samples to be run and the stored method to be used for each. The sequence is divided into a priority sequence (ALS only), subsequences (each of which uses a single method), and post- sequence events Priority sequenceallows you to interrupt a running ALS or valve sequence to analyze urgent samples. (See About the priority sequence on page 115.) Subsequencescontain the stored method number and information that defines a set of samples and calibrators to be analyzed using a particular method. Sampler and/or valve subsequences can be used in the same sequence. Post sequencenames a method to be loaded and run after the last run in the last subsequence. Specifies whether the sequence is to be repeated indefinitely or halted after the last subsequence. Samples in each subsequence are specified as either ALS tray locations or sampling valve positions (gas or liquid sampling valves, often with a stream selection valve). Five sequences with up to five subsequences each can be stored.
About the priority sequence

The priority sequence consists of a single sampler or valve subsequence and a special Use priority parameter, which can be activated at any time, even when a sequence is running. This feature allows you to interrupt a running sequence without having to edit it. If Use priority is On, then:
1 The GC and ALS complete the current run, then the
sequence pauses.
2 The GC runs the priority sequence. 3 The GC resets the Use priority parameter to Off. 4 The main sequence resumes where it paused.
Advanced User Guide
115
To program a sequence
1 Press [Seq]. (Press again, if necessary, to display
subsequence information.)
2 Create a priority sequence, if desired. (See To program a
priority sequence on page 116.) If you might want to use a priority sequence, you must program it now. (Once the sequence starts, you cannot edit it without stopping it.)
3 Scroll to the Method # line of Subseq 1 and enter a method
number. Use 0 for the currently active method, 1 to 9 for the stored methods, or [Off/No] to end the sequence.
4 Press [Mode/Type] to select a valve or injector type. (See
To program a valve subsequence on page 117 or To program an ALS subsequence on page 117.)
5 Create the next subsequence or scroll to Post Sequence.
(See To program post sequence events on page 117.)

6 Save the completed sequence. (See To save a sequence
on page 118.)
To program a priority sequence

2 Scroll to Priority Method # and enter a method number. Use
0 for the currently active method, 1 to 9 for the stored methods, or [Off/No] to end the sequence. Press [Enter]. The active method, 0, will change during the sequence if the subsequences use stored methods. Therefore, method 0 should be chosen for the priority sequence only if all subsequences use method 0.
3 Press [Mode/Type] and select the injector type. 4 Program the ALS subsequence. (See To program an ALS
subsequence on page 117.)

5 Store the completed sequence. (See To save a sequence
on page 118.) Once a priority subsequence exists in a sequence, you can activate it when the urgent samples are ready to be processed by:
2 Scroll to Use Priority and press [On/Yes].
116
Advanced User Guide
When the priority samples are completed, the normal sequence resumes.
To program an ALS subsequence

1 See step 1 through step 3 of To program a sequence on
page 116.
2 Press [Mode/Type] and select the injector type. 3 Enter injector sequence parameters (if using both
injectors, there will be two sets of parameters): Number of Injections/vialthe number of repeat runs from each vial. Enter 0 if no samples are to be injected. Samplesthe range (firstlast) of sample vials to be analyzed.
4 Proceed with step 5 of To program a sequence on
page 116.
To program a valve subsequence

page 116.
2 Press [Mode/Type] and select Valve. 3 Enter the valve sequence parameters (the first three
appear only if a multiposition valve is configured): #inj/positionnumber of injections at each position (099) Position rngfirstlast valve positions to sample (132) Times thru rangenumber of times to repeat the range (199) # injectionsnumber of injections for each sample
4 Proceed with step 5 of To program a sequence on
page 116.
To program post sequence events

page 116.
2 Scroll to the Method # line of Post Sequence and enter a
method number. Use 1 to 9 for the stored methods, or 0 if there is no method to be loaded.
3 Press [On/Yes] at Repeat sequence to keep repeating the
sequence (useful for valve sequences). Otherwise, press
Advanced User Guide
117
[Off/No] to halt the sequence when all subsequences are finished.
To save a sequence
1 Press [Store][Seq]. 2 Enter an identifying number for the sequence. 3 Press [On/Yes] to store the sequence. Alternatively, press
[Off/No] to cancel. A message is displayed if a sequence with the number you selected already exists. Press [On/Yes] to replace the existing sequence or [Off/No] to cancel. Sequences can also be stored from within the stored sequence list ([Seq]) by scrolling to the appropriate sequence number and pressing the [Store] key.
To load a stored sequence

Press [Load][Seq]. Supply the sequence number and press [Enter]. The specified sequence will replace the current active sequence.
To determine sequence status

Press [Seq Control] to display the current status of the active sequence. There are six possible sequence status modes: Start/running Ready wait Paused/resume Stopped Aborted No sequence
To start a sequence
Press [Seq Control], scroll to Start sequence and press [Enter]. The sequence status will change to Running. The sequence continues to run until all subsequences are executed, or until one of the events described under To abort a sequence on page 119 occurs.
118
Advanced User Guide
Ready wait
If a sequence is started but the instrument is not ready (due to oven temperature, equilibration times, etc.), the sequence will not start until all instrument setpoints are ready
To pause and resume a sequence

Press [Seq Control], scroll to Pause sequence, and press [Enter]. The sequence status changes to paused, and you are given the option to resume or stop the paused sequence. The sequence halts when the current sample run is complete. To continue the paused sequence, scroll to Resume sequence and press [Enter]. When a sequence is resumed, it starts with the next sample.
To stop a sequence
A sequence automatically stops at the end of the last active subsequence unless Repeat sequence is On in the Post Sequence events. To stop a running sequence, scroll to Stop sequence and press [Enter]. A stopped sequence can only be restarted from the beginning.
To abort a sequence
When a sequence is aborted, it stops immediately without waiting for the current run to finish. These actions will cause a sequence to abort: A run is stopped by pressing [Stop]. A sampler error occurs producing an error message. The GC detects a configuration mismatch during a method load. A running sequence tries to load an empty method. The sampler is turned off. You can correct the problem and then resume the sequence. The aborted sample run will be repeated.
Advanced User Guide
119
120
Advanced User Guide
6 Checking for Leaks

Preparing the GC for Maintenance 122 To Check for External Leaks 124 To Check for GC Leaks 125 Leaks in Capillary Column (Microfluidic) Fittings 126 To Perform a SS Inlet Pressure Decay Test 127 To Correct Leaks in the Split Splitless Inlet 131 To Perform a Multimode Inlet Pressure Decay Test 132 To Correct Leaks in the Multimode Inlet 136 To Perform a SS Inlet Pressure Decay Test 127 To Correct Leaks in the Packed Column Inlet 141 To Perform a COC Pressure Decay Test 142 To Correct Leaks in the Cool On-Column Inlet 145 To Perform a PTV Pressure Decay Test 146 To Correct Leaks in the PTV Inlet 150 To Perform a VI Pressure Decay Test 151 To Prepare the VI for a Closed System Leak Check 155 To Correct Leaks in the Volatiles Interface 156
121
Checking for Leaks
Preparing the GC for Maintenance

Before most maintenance procedures, the GC must be made ready. The purpose of this preparation is to avoid damage to both the instrument (electronics, columns, etc.) and the user (shocks, burns).
Column and oven preparation

The main hazards here are temperature (burns) and column exposure to air. Cool the oven by changing its setpoint to 35 C. This allows the oven fan to assist cooling. Leave the carrier gas flow On until the oven has cooled. This protects the column from oxygen damage.
Inlet preparation
We are concerned with the possibility of burns and air intrusion into the column. After the oven and columns have cooled, reduce all inlet flows to 0.0 and turn the temperatures Off. For inlet- only maintenance, leave all detectors at their normal setpoints except for the TCD filament, which should be turned Off. If the column is to be removed, cap both ends to keep air out.
Detector preparation
This is another burn hazard area, plus the possibility of damage to the very sensitive electronics. Some detectors (uECD, FPD, NPD) require 12 hours or longer to stabilize from the detector- off condition. To cool the detector, reduce the temperature setpoint to 35 C. Some detectors (FID, NPD, FPD) use high voltages. The high voltage supply is part of the electrometer. Turn it Off to disable the high voltage. The filament in the TCD will be damaged if exposed to air while hot. To protect the filament, turn it Off.
122
Advanced User Guide
Checking for Leaks
Leak Check Tips

When checking for leaks, consider the system in two parts: external leak points and GC leak points. External leak points include the gas cylinder (or gas purifier), regulator and its fittings, supply shutoff valves, and connections to the GC supply fittings. GC leak points include inlets, detectors, column connections, valve connections, and connections between flow modules and inlets/detectors.
WA R N I N G
Hydrogen (H2) is flammable and is an explosion hazard when mixed with air in an enclosed space (for example, a flow meter). Purge flowmeters with inert gas as needed. Always measure gases individually. Always turn off detectors to prevent flame/bead autoignition.
WA R N I N G
Hazardous sample gases may be present.
Electronic leak detector capable of detecting the gas type 7/16, 9/16, and 1/4- inch wrenches for tightening Swagelok and column fittings
2 Check any potential leak points associated with any
maintenance recently performed.

3 Check GC fittings and connections that undergo thermal
cycling, since thermal cycling tends to loosen some fitting types. Use the electronic leak detector to determine if a fitting is leaking. Start by checking any newly made connections. Remember to check connections in the gas supply lines after changing traps or supply cylinders.
Advanced User Guide
123
Checking for Leaks
To Check for External Leaks

Check for leaks at these connections:
Gas supply bulkhead fittings Gas cylinder fitting Regulator fittings Traps Shut- off valves T- fittings Perform a pressure drop test.
1 Turn off the GC. 2 Set the regulator pressure to 415 kPa (60 psi). 3 Fully turn the regulator knob counterclockwise to shut
the valve.
4 Wait 5 minutes. If there is a measurable drop in pressure,
there is a leak in the external connections. No drop in pressure indicates that the external connections are not leaking.
124
Advanced User Guide
Checking for Leaks
To Check for GC Leaks

Check for leaks at these connections: Inlet septum, septum head, liner, split vent trap, split vent trap line, and purge vent fittings Column connections to inlets, detectors, valves, splitters, and unions Fittings from the flow modules to the inlets, detectors, and valves Column adapters Agilent capillary flow fittings
Advanced User Guide
125
Checking for Leaks
Leaks in Capillary Column (Microfluidic) Fittings

For capillary column fittings, a leak usually indicates that the fitting has been overtightened. Unless the fitting is obviously loose, do not tighten it further. Instead, remove the connection, trim the column end, and install it again. Also inspect the plate and connection for a broken column tip.
126
Advanced User Guide
Checking for Leaks
To Perform a SS Inlet Pressure Decay Test

The pressure decay test checks for leaks from the inlet flow module up to the column fitting. After performing maintenance, first check for leaks in externally accessible areas. See To Check for External Leaks. If a leak is known to exist, check the externally accessible inlet fittings first, especially any connection that has seen recent maintenance, such as the septum nut, column adapter, column connection, and so forth. The pressure decay leak test described below requires removing the column and capping the inlet column fitting. This test can/cannot find the following types of leaks:
The test can find leaks at the: septum septum nut liner O-ring seal gold seal/washer and reducing nut inlet body flow manifold split vent valve flow manifold septum purge valve split vent tubing and trap septum purge tubing seals within the tubing between the inlet flow module and the inlet body
The test cannot find leaks at the: column fitting gas supply bulkhead fittings to the flow module tubing and connections in a transfer line connected to the inlet internal leaks in an EPC module (septum purge valve)
1 Gather the following (see Consumables and parts for the
split/splitless inlet): No- hole ferrule 1/4- inch wrench Heat- resistant gloves (if the inlet is hot) Column nut
Advanced User Guide
127
Checking for Leaks
New septum O- ring ECD/TCD Detector plug (part no. 5060- 9055)
2 Load the inlet maintenance method and wait for the GC
to become ready.
3 Remove the column, if installed. 4 Plug the column fitting with a column nut and a no- hole
ferrule.
5 Remove the old septum and replace it with a new one.
See To change the septum on the split/splitless inlet.

6 Inspect the O- ring and replace it if it is hard and brittle
or cracked. See To change the liner and O- ring on the split/splitless inlet.
7 Set the inlet to Split Mode. 8 Configure the column as Inlet: Unspecified. 9 Set the inlet temperature to 70 C. 10 Set the Total flow to 60 mL/min. 11 Enter a pressure setpoint of 25 psi (172 kPa). Make sure
that the pressure supplied to the GC is at least 10 psi (70 kPa) higher than the inlet pressure.
12 If pressure cannot be achieved, there is either a large leak
or the supply pressure is too low.

13 Set the Septum purge flow to 3.0 mL/min. 14 Cap the septum purge fitting with the ECD/TCD detector
plug.
128
Advanced User Guide
Checking for Leaks
Back inlet split vent Front inlet split vent
Back inlet purge vent
Front inlet purge vent
Front purge vent shown plugged
15 From the keypad, press [Service Mode]. Select Diagnostics >
Front or Back Inlet > Pneumatics Control > Septum Purge control.
16 Scroll to the Constant duty cycle and enter 50. Wait 10
seconds.
17 Press [Front or Back Inlet]. Scroll to Pressure and press
Off/No.
18 Quickly turn off the carrier gas supply at its source. 19 Monitor the pressure for 10 minutes. Use the timer by
pressing [Time] and [Enter]. A pressure drop of less than 0.5 psig (0.05 psi/min or less; 3.4 kPa or 0.34 kPa/min) is acceptable.
Advanced User Guide
129
Checking for Leaks
If the pressure drops much faster than the acceptable rate, see To Correct Leaks in the Split Splitless Inlet. Retest. Note that liner size impacts pressure drop. An inlet with a smaller volume liner does not tolerate as large a leak rate as an inlet with a larger volume liner.
20 After the inlet passes the test, restore the GC to
operating condition. Remove any caps/plugs. Reinstall the column. Restore the correct column configuration. Load the operating method.
130
Advanced User Guide
Checking for Leaks
To Correct Leaks in the Split Splitless Inlet

If the inlet fails a pressure decay test, check the following: Check the caps/plugs used in the testmake sure each is correctly installed and tight. If you performed the leak test after performing maintenance, check for proper installation of the part(s) handled during the maintenance. Check the tightness of the septum nut. See To change the septum on the split/Splitless inlet. Check the septum. Replace if old or damaged. Check the insert assembly installation. Check the liner and liner O- ring. See To change the liner and O- ring on the split/splitless inlet. If you changed the gold seal, verify correct installation. See To replace the gold seal on the split/splitless inlet. If these items do not resolve the problem, contact Agilent for service.
Advanced User Guide
131
Checking for Leaks
To Perform a Multimode Inlet Pressure Decay Test

The test can find leaks at the: septum septum nut liner O-ring seal inlet body flow manifold split vent valve flow manifold septum purge valve split vent tubing and trap septum purge tubing seals within the tubing between the inlet flow module and the inlet body
The test cannot find leaks at the: column fitting gas supply bulkhead fittings to the flow module tubing and connections in a transfer line connected to the inlet
Multimode inlet): No- hole ferrule 1/4- inch wrench Heat- resistant gloves (if the inlet is hot) Column nut New septum O- ring
132
Advanced User Guide
Checking for Leaks
ECD/TCD Detector plug (part no. 5060- 9055)

to become ready.
ferrule.
See To change the septum on the multimode inlet.

or cracked. See To change the liner and O- ring on the Multimode inlet.
7 Set the inlet to Split Mode. 8 Configure the column as Inlet: Unspecified. 9 Set the inlet temperature to 70 C. 10 Set the Total flow to 60 mL/min. 11 Enter a pressure setpoint of 25 psi (172 kPa). Make sure

plug.
Advanced User Guide
133
Checking for Leaks
seconds.
Off/No.
134
Advanced User Guide
Checking for Leaks
If the pressure drops much faster than the acceptable rate, see To Correct Leaks in the Multimode Inlet. Retest. Note that liner size impacts pressure drop. An inlet with a smaller volume liner does not tolerate as large a leak rate as an inlet with a larger volume liner.
Advanced User Guide
135
Checking for Leaks
To Correct Leaks in the Multimode Inlet

If the inlet fails a pressure decay test, check the following: Check the caps/plugs used in the testmake sure each is correctly installed and tight. If you performed the leak test after performing maintenance, check for proper installation of the part(s) handled during the maintenance. Check the tightness of the septum nut. See To change the septum on the Multimode inlet. Check the septum. Replace if old or damaged. Check the insert assembly installation. Check the liner and liner O- ring. See To change the liner and O- ring on the Multimode inlet. If these items do not resolve the problem, contact Agilent for service.
136
Advanced User Guide
Checking for Leaks
To Perform a PP Inlet Pressure Decay Test

The test can find leaks at the: septum septum nut glass insert O-ring seal adapter and ferrule inlet body top insert weldment seals within the tubing between the inlet flow module and the inlet body
The test cannot find leaks at the: column fitting gas supply bulkhead fittings to the flow module
purged packed inlet): No- hole ferrule 1/4- inch wrench 7/16- inch wrench Heat- resistant gloves (if the inlet is hot) 9/16- inch wrench 1/8- and 1/4- inch Swagelok caps ECD/TCD Detector plug (part no. 5060- 9055)
to become ready.
Advanced User Guide
137
Checking for Leaks
3 Remove the column, if installed. 4 Plug the column fitting.
If the capillary column adapter is installed, use a column nut and a no- hole ferrule If a 1/8- inch packed column adapter is installed, use a 1/8- inch Swagelok cap (5180- 4121). If a 1/4- inch packed column adapter is installed, use a 1/4- inch Swagelok cap (5180- 4120)
See To change the septum on the purged packed inlet.

or cracked. See To change the O- ring on the purged packed inlet.

7 If unsure of the quality of the adapter ferrule, replace it.
See To change the glass insert on a PP inlet.

8 Configure, but do not install, a capillary column to put
the inlet in pressure control mode.

9 Set the inlet temperature to 100 C. 10 Enter a pressure setpoint of 25 psi (172 kPa). Make sure

plug.
138
Advanced User Guide
Checking for Leaks
seconds.
Off/No.
Advanced User Guide
139
Checking for Leaks
If the pressure drops much faster than the acceptable rate, see To Correct Leaks in the Packed Column Inlet. Retest.
140
Advanced User Guide
Checking for Leaks
To Correct Leaks in the Packed Column Inlet

If the inlet fails a pressure decay test, check the following: Check the caps/plugs used in the testmake sure each is correctly installed and tight. If you performed the leak test after performing maintenance, check for proper installation of the part(s) handled during the maintenance. Check the tightness of the septum nut. See To change the septum on the purged packed inlet. Check the septum. Replace if old or damaged. Check that the top insert weldment is installed tightly. Replace the O- ring. See To change the O- ring on the purged packed inlet. Also check the glass insert. See To change the glass insert on a PP inlet. Replace the ferrule seal on the adapter. If these items do not resolve the problem, contact Agilent for service.
Advanced User Guide
141
Checking for Leaks
To Perform a COC Pressure Decay Test

The pressure decay test checks for leaks from the inlet flow module up to the column fitting. After performing maintenance, first check for leaks in externally accessible areas. See To Check for External Leaks. If a leak is known to exist, check the externally accessible inlet fittings first, especially any connection that has seen recent maintenance, such as the septum nut, column adapter, column connection, and so forth. See To Check for External Leaks. The pressure decay leak test described below requires removing the column and capping the inlet column fitting. This test can/cannot find the following types of leaks:
The test can find leaks at the: septum septum nut or cooling tower seals within the tubing between the inlet flow module and the inlet body inlet body
The test cannot find leaks at the: column fitting gas supply bulkhead fittings to the flow module
COC inlet): No- hole ferrule 1/4- inch wrench Heat- resistant gloves (if the inlet is hot) Column nut New septum ECD/TCD Detector plug (part no. 5060- 9055)
to become ready.
3 Remove the column, if installed. 4 Plug the column fitting with a column nut and no- hole
ferrule.
142
Advanced User Guide
Checking for Leaks
See To change a septum on the COC inlet.

6 Enter a pressure setpoint of 25 psi (172 kPa). Make sure
7 Wait 5 minutes for the pressure to equilibrate. If pressure
cannot be achieved, there is either a large leak or the supply pressure is too low.
plug.
Back inlet split vent Front inlet split vent Front inlet purge vent Back inlet purge vent
Advanced User Guide
143
Checking for Leaks
seconds.
Off/No.
pressing [Time] and [Enter]. A pressure drop of less than 1.0 psig (0.1 psi/min or less; 6.9 kPa or 0.69 kPa/min) is acceptable. If the pressure drops much faster than the acceptable rate, see To Correct Leaks in the Cool On- Column Inlet. Retest.
144
Advanced User Guide
Checking for Leaks
To Correct Leaks in the Cool On-Column Inlet

If the inlet fails a pressure decay test, check the following: Check the caps/plugs used in the testmake sure each is correctly installed and tight. If you performed the leak test after performing maintenance, check for proper installation of the part(s) handled during the maintenance. Check the tightness of the septum nut or cooling tower assembly. See To change a septum nut or cooling tower and septum on a COC inlet. Check the septum. Replace if old or damaged. If these items do not resolve the problem, contact Agilent for service.
Advanced User Guide
145
Checking for Leaks
To Perform a PTV Pressure Decay Test

The test can find leaks at the: septum septum nut liner O-ring seal gold seal/washer and reducing nut inlet body flow manifold split vent valve flow manifold septum purge valve split vent tubing and trap septum purge tubing seals within the tubing between the inlet flow module and the inlet body
PTV inlet): No- hole ferrule 1/4- inch wrench Heat- resistant gloves (if the inlet is hot) Column nut New septum
146
Advanced User Guide
Checking for Leaks
New Graphpak 3D ferrule and liner ECD/TCD Detector plug (part no. 5060- 9055)
to become ready.
ferrule.
5 If using the septum head, and the quality of the septum
(or Microseal) and GRAPHPACK- 3D ferrule on the glass liner are unknown, replace them now. See To change the septum on the PTV inlet and To change the liner on the PTV inlet.
6 Set the inlet to Split Mode. 7 Configure the column as 0 length. 8 Set the inlet temperature to 100 C. 9 Set the Total flow to 60 mL/min. 10 Enter a pressure setpoint of 25 psi (172 kPa). Make sure

plug.
Advanced User Guide
147
Checking for Leaks
seconds.
Off/No.
148
Advanced User Guide
Checking for Leaks
If the pressure drops much faster than the acceptable rate, see To Correct Leaks in the PTV Inlet. Retest. Note that liner size impacts pressure drop. An inlet with a smaller volume liner does not tolerate as large a leak rate as an inlet with a larger volume liner.
Advanced User Guide
149
Checking for Leaks
To Correct Leaks in the PTV Inlet

If the inlet fails a pressure decay test, check the following: Check the caps/plugs used in the testmake sure each is correctly installed and tight. If you performed the leak test after performing maintenance, check for proper installation of the part(s) handled during the maintenance. If using a septum head, check the tightness of the septum nut. See To change the septum on the PTV inlet. If using a septum head, check the septum. Replace if old or damaged. Check that the septumless- or septum- head assembly is installed tightly. Replace the liner and Graphpak 3D ferrule. See To change the liner on the PTV inlet. Check the Graphpak adapter seal against the inlet body. Replace the silver seal and reinstall the adapter if needed. See To replace the inlet adapter for the PTV inlet. If using the septumless head, check for leaks around the guide cap. Replace the Teflon ferrule in the guide cap. See To replace the Teflon ferrule on a PTV inlet. Check for leaks at the split vent trap. Tighten as necessary. Replace the split vent trap filter and O- rings. See To replace the filter in the PTV inlet split vent line. If these items not resolve the problem, contact Agilent for service.
150
Advanced User Guide
Checking for Leaks
To Perform a VI Pressure Decay Test

The pressure decay test checks for leaks from the inlet flow module up to the column fitting. Initially test the VI with a sampling system installed. If the system fails the leak test, then isolate the VI from the sampler as described in To Prepare the VI for a Closed System Leak Check on page 155. After performing maintenance, first check for leaks in externally accessible areas. See To Check for External Leaks. If a leak is known to exist, check the externally accessible inlet fittings first, especially any connection that has seen recent maintenance, such as the column connection, split vent line, and so forth. The pressure decay leak test described below requires removing the column and capping the inlet column fitting. This test can/cannot find the following types of leaks:
The test can find leaks at the: sampler connection pressure sensing line connection to the interface split vent line connection to the interface the connected samplers entire sample flow path flow manifold split vent valve flow manifold septum purge valve split vent tubing and trap
VI): No- hole ferrule 1/4- inch wrench Heat- resistant gloves (if the inlet is hot) Long column nut ECD/TCD Detector plug (part no. 5060- 9055)
Advanced User Guide
151
Checking for Leaks
to become ready.
ferrule.
5 Set the inlet to Split Mode. 6 Configure the column as 0 length. 7 Set the inlet temperature to 100 C. 8 Set the Total flow to 60 mL/min. 9 Enter a pressure setpoint of 25 psi (172 kPa). Make sure

plug.
Back inlet split vent Front inlet split vent Front inlet purge vent Back inlet purge vent
152
Advanced User Guide
Checking for Leaks
seconds.
Off/No.
pressing [Time] and [Enter]. The pressure should drop approximately 1 psi (6.9 kPa) during the first 1 to 2 minutes. After an initial pressure drop of about 1 psi, the pressure should not drop more than 0.03 psi/min (0.21 kPa/min). If the pressure drop is 0.03 psi/min or less, you can consider the interface- gas sampler system leak- free. If the pressure drops faster than the acceptable rate, you must check the interface and sampler systems separately to determine the source of the leak. See To Prepare the VI for a Closed System Leak Check to create a closed flow system, then return to this section and complete steps 10 to 15. If you find a leak in the interface, refer to To Correct Leaks in the Volatiles Interface. If the interface is leak- free, pressure check the sampling device. See the operating manual for your sampler for instructions.
18 After the VI passes the test, restore the GC to operating
condition. Remove any caps/plugs. If needed, reconnect the sampling device. Reinstall the column. Restore the correct column configuration.
Advanced User Guide
153
Checking for Leaks
Load the operating method.
154
Advanced User Guide
Checking for Leaks
To Prepare the VI for a Closed System Leak Check

To leak check the interface independently of the gas sampling device, you must disconnect the sampler from the interface to isolate the interface flow system from the sampler.
WA R N I N G
Be careful! The oven and/or inlet may be hot enough to cause burns. If either is hot, wear heat-resistant gloves to protect your hands.
1/16- inch nut for transfer line Ferrule for transfer line Heat- resistant gloves (if the inlet is hot)
2 Disconnect the transfer line from the interface. 3 Disconnect the carrier line from the sampler. 4 Prepare the end of the carrier line using a 1/16- inch male
nut and ferrule.

5 Connect the carrier line to the interface where you
removed the transfer line and tighten the nut finger tight. Tighten an additional 1/4 to 1/2 turn with the 1/4- inch wrench.
6 Return to To Perform a VI Pressure Decay Test and
repeat steps 9 to 15.
Advanced User Guide
155
Checking for Leaks
To Correct Leaks in the Volatiles Interface

If the inlet fails a pressure decay test, check the following: The caps and plugs used in the testmake sure each is correctly installed and tight. If you performed the leak test after performing maintenance, check for proper installation of the part(s) handled during the maintenance. The split vent and pressure sensing connections at the interface. The sampler connection to the interface. The sampler. If these items do not resolve the problem, contact Agilent for service.
156
Advanced User Guide
7 Flow and Pressure Modules

About Flow and Pressure Control 158 Maximum operating pressure 158 PIDs 159 Inlet Modules 160 Detector Modules 161 Pressure Control Modules 162 Auxiliary Pressure Controllers 165 Restrictors 166 1. Using an Aux epc channel to supply purge gas to a splitter 167 2. Using the PCM channels 167
157
About Flow and Pressure Control

The GC uses four types of electronic flow or pressure controllers; inlet modules, detector modules, pressure control modules (PCMs), and auxiliary pressure controllers (Aux EPCs). All of these modules mount in the slots at the top rear of the GC. The slots are identified by numbers, as shown here.
Slot 5 Slot 6
Slot 3 Slot 4 Back of GC
Slot 1 Slot 2 Split vent traps and valves
When a module is installed in a slot, it must be connected to the communications buss that runs underneath it. Each branch of the buss has an identifying label near the connector. The proper branch must be connected to the module for the firmware to recognize it. Branch/slot assignments are:
EPC5 EPC6
EPC3 EPC4
EPC1 EPC2 Back of GC
Split vent traps and valves
If a detector is mounted in the left side carrier (as seen from the front side of the oven), it is controlled by EPC6. An extension cable connects to EPC6, runs across the top of the oven just in front of the top row of slots, and passes through an opening into the detector carrier.
Maximum operating pressure

The pneumatics modules of the GC will stand over 250 psi pressure, but may not function reliably. We recommend a maximum continuous operating pressure of 170 psi to avoid excessive wear and leaks.
158
Advanced User Guide
PIDs
The behavior of a pressure control module is governed by a set of three constants, called P (proportional), I (integral), and D (differential). Certain gases or special applications (such as QuickSwap, headspace vial pressurization, or splitter and backflush applications) require different PIDs than those provided at the factoory. If you need to update or change the pneumatic PID values for an application, use the utility program on the documentation and utility DVD provided with the GC. The table summarizes custom PID values required for selected applications. Note that if you are updating an AUX EPC module, you will need to change the frit for the channel used. Table 23 PIDs and frits
Application QuickSwap Purged splitter and Deans Switch when using backflush Purged splitter and Deans Switch Headspace vial pressurization Headspace sampling loop Module AUX EPC AUX EPC AUX EPC AUX EPC PCM in backpressure control AUX frit Brown, 1 ring No color or rings Brown, 1 ring No color or rings Select Available PID Values Quickswap Quickswap Standard AUX_EPC_Headspace PCM_Headspace
Advanced User Guide
159
Inlet Modules
These modules are used with specific inlets. They provide a controlled flow or pressure of carrier gas to the inlet and control the septum flow rate. Module locations depend on the type of module and the length of the tubing connecting it to the inlet. If you have a Front inlet, its flow module must go in Slot 1. If you have a Back inlet, its flow module must go in Slot 2.
160
Advanced User Guide
Detector Modules
These are specific to the detector with which they are supplied, and differ according to the needs of that detector. For example, the FID module must supply controlled amounts of air, hydrogen, and makeup gas. The TCD module supplies the reference and makeup gases, but includes the reference switching valve that is essential to detector operation. Module locations depend on the type of module and the length of the tubing connecting it to the detector. If you have a Front detector, its flow module must go in Slot 3. If you have a Back detector, its flow module must go in Slot 4. If you have a TCD detector mounted on the left side of the GC, its flow module mounts in a special bracket near the detector.
Advanced User Guide
161
Pressure Control Modules

The PCM is a general purpose module with two independent control channels, designated 1 and 2. The general name of a PCM module is PCM #, where the # (actually, a letter) identifies the PCM (there can be up to 3 installed). The two channels are not identical. Channel 1 is a simple forward- pressure regulated channel that maintains constant flow through a fixed restrictor.
Channel 2 may be used either as a forward- pressure regulator or as a backpressure regulator, simply by reversing the input and output connections. The back
162
Advanced User Guide
pressure mode can be very useful with a gas sampling valve, where it ensures that the sample pressure in the loop remains constant.
For channel 1, gas input is via a threaded fitting. Gas output is via a coil of metal tubing with a Swagelok fitting on the end. For channel 2, the connections are the same as for channel 1 if channel 2 is to be used as a forward- pressure regulator. They are reversedextra fittings/adapters will be neededif it is to be used as a backpressure regulator. PCMs can be installed in several locations: In slot 1. The name is PCM A. In slot 2. The name is PCM B.
Advanced User Guide
163
In slot 5. If there are no PCMs in slots 1 and 2, the name is PCM A. If another PCM is installed in either slot 1 or 2, the PCM in slot 5 takes the name that is not being used (A or B). If PCMs are installed in both slots 1 and 2, the name is PCM C. In slot 6. The name is always PCM C.
PCM A or B PCM C
Slot 3 Slot 4
PCM A PCM B Back of GC Split vent trap and valve
Both channels of a PCM are controlled by the same parameter list. The first two lines refer to channel 1, the remaining lines refer to channel 2.
164
Advanced User Guide
Auxiliary Pressure Controllers

The Auxiliary Pressure Controller (Aux epc) is also a general purpose device. It has three independent forward- pressure regulated channels. Channels are designated by numbers 1 through 9 (there can be up to 3 Aux epcs), depending on where the module is installed. If an auxiliary channel is specified as the Inlet during column configuration, that channel allows run time programming and three- ramp flow or pressure programming. Gas input is via threaded fittings. Gas output is via coils of metal tubing with Swagelok fittings on the ends. As you look at the module from the back of the GC, the channels are numbered from left to right according to this scheme: In slot 6. The name is Aux epc #, where # is 1, 2, or 3 and identifies the channel. In slot 5. The name is Aux epc #, where # is 4, 5, or 6 and identifies the channel. In slot 4. The name is Aux epc #, where # is 7, 8, or 9 and identifies the channel. In the third detector side of the GC. The name is Aux epc #, where # is 7, 8, or 9 and identifies the channel.
Aux epc 4, 5, 6
Slot 3
Slot 1 Slot 2 Split vent trap and valve
Aux epc 1, 2, 3 Aux epc 7, 8, 9

Back of GC
Advanced User Guide
165
Restrictors
Both PCMs and auxiliary channels are controlled by pressure setpoints. To work properly, there must be adequate flow resistance downstream of the pressure sensor. Each channel provides a frit- type restrictor. Four frits are available. Table 24 Auxiliary channel frits
Frit marking Three blue rings Two red rings One brown ring None (brass tube) Flow resistance High Medium Low Zero Flow characteristic 3.33 0.3 SCCM @ 15 PSIG 30 1.5 SCCM H2 @ 15 PSIG 400 30 SCCM AIR @ 40 PSIG No restriction Often used with FID Air, QuickSwap, Splitter, Deans Switch FID Hydrogen NPD Hydrogen Headspace vial pressurization
The brown ring frit is in all channels in the AUX epc when the instrument is shipped. No frit ships in the PCM Aux channel. When installing or replacing a frit, always use a new O- ring (5180- 4181, 12/pk).
Selecting a frit
The frits change the control range of the channels. The objective is to find a frit that allows the required range of flows at reasonable source pressures. For an auxiliary channel ordered as an option (part of the GC order), use the frit supplied by the factory. For an auxiliary channel ordered as an accessory (separate from the GC order), see the instruction information supplied with the accessory. For a non- Agilent instrument, you must experiment to find the appropriate frit. When you change a frit, you change the physical characteristics of the channel. It may be desirable (or necessary) to change the PID constants for that channel. See PIDs on page 159.
166
Advanced User Guide
Examples
1. Using an Aux epc channel to supply purge gas to a splitter
An Aux epc channel operates only in the forward- pressure mode; it provides a constant pressure at its outlet. It is used to provide gas to some other device, such as a splitter with a makeup gas input.
Split/splitless inlet
Aux EPC
ECD
FPD
MSD
0.507 m x 0.10 mm x 0 m
0.532 m x 0.18 mm x 0 m
1.444 m x 0.18 mm x 0 m
30 m x 0.25 mm x 0.25 m HP-MS5
In this configuration, the gas eluting from the column is divided among three detectors. Because the resulting flows can be quite small, makeup gas is added at the splitter. An Aux epc channel provides it. Assume that we are using channel Aux epc 1 as the makeup source. The gas is plumbed to the leftmost (as seen from the back of the GC) fitting on the proper module. The outlet tubing for this channel goes to the splitter inside the ovenan extension tube may be needed to reach this far. The medium frit is probably appropriate for this application. Rather than have the makeup gas flowing all the time, consider turning it on and off with run time commands.
2. Using the PCM channels

The two channels in a PCM are different. Channel 1 is used to supply a pressure. Channel 2 may be used in the same way, but can also be used to maintain a pressure by reversing the input and output connections.
Advanced User Guide
167
Channel 1: Forward-pressure only

This is identical to the carrier gas channel for the packed column inlet.
Channel 2: Two-way channel

If gas is supplied at the threaded connection and delivered by the tubing, this operates the same as channel 1. But the connections can be reversedrequiring some fittingsso that it will maintain the gas supplied to it at a fixed pressure. In this mode it behaves as a controlled leak. This can be used to maintain the gas in a gas sampling valve at a fixed pressure, even if the supply varies somewhat. The result is improved reproducibility in sample amount. The figure shows the connections with the valve in the Load position.
To column
Carrier in Back-pressure regulation
Valve
PS
Sample in Threaded connection Sample out
Vent connection
168
Advanced User Guide
8 Inlets
Using Hydrogen 171 Inlet Overview 172 Carrier Gas Flow Rates 173 About Gas Saver 174 Pre Run and Prep Run 176 Auto Prep Run 177 About Heaters 178 About the Split/Splitless Inlet 180 Split/Splitless inlet split mode overview 181 Split/Splitless inlet splitless mode overview 182 The S/SL inlet pulsed split and splitless modes 183 Split/Splitless inlet split mode minimum operating pressures 184 Selecting the correct S/SL inlet liner 185 Vapor Volume Calculator 187 Selecting parameters for the S/SL splitless mode 188 About the Multimode Inlet 191 Septum tightening (MMI) 191 Heating the MMI 192 Cooling the MMI 192 MMI split mode minimum operating pressures 193 Selecting the correct MMI liner 194 Vapor Volume Calculator 195 MMI split and pulsed split modes 195 MMI splitless and pulsed splitless modes 199 MMI solvent vent mode 205 MMI Direct Mode 213 To develop a MMI method that uses large volume injection 214 Multiple injections with the MMI 217 About the Cool On-Column Inlet 231 Retention gaps 232 COC inlet temperature control 232 Setting COC inlet flows/pressures 233 About the PTV Inlet 235 PTV sampling heads 235 Heating the PTV inlet 236
169
Inlets
Cooling the PTV inlet 237 PTV inlet split and pulsed split modes 237 PTV inlet splitless and pulsed splitless modes 241 PTV inlet solvent vent mode 248 To develop a PTV method that uses large volume injection 256 Multiple injections with the PTV inlet 259 About the Volatiles Interface 265 About the VI split mode 267 About the VI splitless mode 271 About the VI direct mode 276 Preparing the Interface for Direct Sample Introduction 279 Setting parameters for the VI direct mode 282
170
Advanced User Guide
Inlets
Using Hydrogen
WA R N I N G When using hydrogen (H2), as the carrier gas, be aware that hydrogen (H2) gas can flow into the oven and create an explosion hazard. Therefore, be sure that the supply is off until all connections are made, and ensure that the inlet and detector column fittings are either connected to a column or capped at all times when hydrogen (H2) gas is supplied to the instrument.
WA R N I N G
Hydrogen (H2) is flammable. Leaks, when confined in an enclosed space, may create a fire or explosion hazard. In any application using hydrogen (H2), leak test all connections, lines, and valves before operating the instrument. Always turn off the hydrogen (H2) supply at its source before working on the instrument.
Advanced User Guide
171
Inlets
Inlet Overview
Table 25
Inlet Split/splitless
Comparing inlets
Column Capillary Mode Split Pulsed split Splitless Pulsed splitless Sample concentration High High Low Low High High Low Low Low Comments Useful with large injections Useful with large injections Sample to column Very little Very little All All
Multimode
Capillary
Split Pulsed split Splitless Pulsed splitless Solvent vent
Very little Very little All All Multiple injections Most concentrate analytes and vent solvent All
Direct Cool on-column Capillary n/a Low or labile Minimal discrimination and decomposition OK if resolution not critical
All
Packed column
Packed Large capillary Capillary
n/a n/a Split Pulsed split Splitless Pulsed splitless Solvent vent
Any Any High High Low Low Low
All All
Programmed temperature vaporization
Very little Very little All All Multiple injections Most concentrate analytes and vent solvent Lowest dead volume Max flow = 100 mL/min All Very little All
Volatiles interface (for use with external volatiles sampler)
Capillary
Direct Split Splitless
Low High Low
172
Advanced User Guide
Inlets
Carrier Gas Flow Rates

The flow rates in Table 26 are recommended for all column temperatures. Table 26
Column type
Column size and carrier flow rate

Column size Carrier flow rate, mL/min Hydrogen Helium 30 60 0.5 1.0 2.0 2.5 3.2 5.3 0.4 0.8 1.6 2.0 2.6 4.2 Nitrogen 20 40 n/a n/a 0.25 0.5 0.75 1.5
Packed
1/8-inch 1/4-inch
Capillary
0.05 mm id 0.10 mm id 0.20 mm id 0.25 mm id 0.32 mm id 0.53 mm id
Advanced User Guide
173
Inlets
About Gas Saver

Gas saver reduces carrier flow from the split vent after the sample is on the column. It applies to the Split/Splitless and PTV inlets (all modes) and to the split and splitless modes of the Volatiles Interface. It is most useful in split applications. Column head pressure and flow rate are maintained, while purge and split vent flows decrease. Flowsexcept column flowremain at the reduced level until you press [Prep Run].
[Start] Split mode Split vent flow mL/min Gas saver time, 3 min
50 40 30
[Prep Run]
Regular flow Run ends
20 Gas saver flow 10 -2 -1 0

[Start] Splitless mode Split vent flow mL/min
Gas saver flow
Time, min Gas saver time, 5 min Purge time, 2 min Purge flow Gas saver flow Run ends
50 40 30
[Prep Run]
20 Gas saver flow 10 -2 -1 0 1 2 3 4 5
Time, min
The pulsed modes of the split/splitless and PTV inlets are similar except for the pressure pulse starting at [Prep Run] and ending at Pulse time. The solvent vent mode of the PTV is more complex; see PTV inlet solvent vent mode on page 248.
To use gas saver

1 Press [Front Inlet] or [Back Inlet]. 2 Turn gas saver On. 3 Set Gas saver flow. It must be at least 15 mL/min greater
than the column flow.
174
Advanced User Guide
Inlets
4 If in split mode, set Saver time after injection time. In all
other modes, set after Purge time.
Advanced User Guide
175
Inlets
Pre Run and Prep Run

With some inlets and operating modes, certain instrument setpoints are different between runs than during an analysis. To restore the setpoints for injection, you must place the GC into the Pre Run state. You must use the Pre Run state when: Using gas saver with any inlet. Using splitless mode with any inlet. Using a pressure pulse mode with any inlet. Using the solvent vent mode of the PTV inlet. Using the direct or splitless mode of the Volatiles Interface. There are three ways to begin Pre Runmanually (press [Prep Run] before each run), automatically (for Agilent samplers), or using Auto Prep Run (for non- Agilent samplers). The three methods are discussed below. During the Pre Run state: The Pre Run light blinks and Not Ready is on. Setpoints change to the correct values for injection. Inlet, detector, and oven equilibration times begin. When all equilibration times expire, the Pre Run light is on steadily. When all criteria for a run are met, the Not Ready light turns off. The GC is now ready for sample injection.
The [Prep Run] key

Press [Prep Run] before you inject a sample manually. The GC enters the Pre Run state. When the Pre Run light is steady and the Not Ready light goes off, begin the analysis.
Agilent samplers
If you are using an Agilent automatic sampling system, the [Prep Run] function is automatic. Start the sampler. It generates the [Prep Run] function, When all the setpoints are reached and the GC becomes Ready, sample injection begins.
176
Advanced User Guide
Inlets
Non-Agilent samplers
With most automatic injection systems, you do not need to use the [Prep Run] key. If your sampler or automation controller (for example, an integrator or workstation) does not support the [Prep Run] function, you must set the GC to Auto Prep Run.
Auto Prep Run

To set this parameter, usually for a non- Agilent integrator, workstation, or other controlling device:
1 Press [Config] to view a list of configurable parameters. 2 Scroll to Instrument and press [Enter]. 3 Scroll to Auto prep run and press [On/Yes].
Advanced User Guide
177
Inlets
About Heaters
Inlets (and detectors, valve boxes, etc.) are heated. There are six heater connectors on the GC mainframe, located as shown here:
Front of GC
Near top right corner of front detector board Near top right corner of back detector board Left end of valve bracket Right end of valve bracket
Near front inlet
4 2 5 6 Near back inlet
All heater connectors are square, 4- conductor receptacles mounted on brackets. The next table describes the heaters that are available for each module. Table 27
Module Front inlet Back inlet Front detector Back detector Aux detector 1 Aux detector 2 PCM A PCM B PCM C AUX 1,2,3 AUX 4,5,6 AUX 7,8,9
Heater connectors by module

Available heater connectors 1 or None 2 or None 3 or 5 4 or 6 5 or 6 or 2 None 5 or 6 or 1 or 2 5 or 6 or 1 or 2 5 or 6 or 1 or 2 None None None
178
Advanced User Guide
Inlets
Table 27
Module Valve box Aux heater 1 Aux heater 2
Heater connectors by module (continued)

Available heater connectors 5 or 6 or Both 5 6
Front FPD uses heater connectors 3 and 5. Back FPD uses heater connectors 4 and 6. FPDs can be configured for one or two heater versions.
Advanced User Guide
179
Inlets
About the Split/Splitless Inlet

This inlet is used for split, splitless, pulsed splitless, or pulsed split analyses. You can choose the operating mode from the inlet parameter list. The split mode is generally used for major component analyses, while the splitless mode is used for trace analyses. The pulsed splitless and pulsed split modes are used for the same type of analyses as split or splitless, but allow you to inject larger samples.
Septum tightening (S/SL)

Septum retainer nuts must be tightened enough to obtain a good gas seal, but not so much as to compress the septum and make it difficult to push a syringe needle through it. For the standard septum retainer nut, an internal spring in the septum retainer applies pressure to the septum. For inlet pressures up to 100 psi, tighten the retainer until the C- ring lifts about 1 mm above the top surface. This is adequate for most situations.
1 mm
With higher inlet pressures, tighten the septum retainer until the C- ring stops turning, indicating that the retainer is in firm contact with the septum. If using a Merlin Microseal septum, finger tighten the septum nut, until snug (not loose). The pressure capacity depends on the duckbill seal used.
Standard and high-pressure versions of the S/SL inlet

The standard split/splitless inlet is rated to 100 psi pressure at the inlet. It is appropriate for most columns. The high- pressure inlet is rated to 150 psi pressureit is useful with very small diameter capillary columns that offer considerable resistance to gas flow. Recommended source pressures are 120 psi and 170 psi respectively.
180
Advanced User Guide
Inlets
To determine the version that you have, press [Front Inlet] or [Back Inlet], scroll to the Pressure line, and press the [Info] key. The display will show the pressure range for the inleteither 1 to 100 psi (for the standard version) or 1 to 150 psi (for the high- pressure version).
Split/Splitless inlet split mode overview

During a split injection, a liquid sample is introduced into a hot inlet where it vaporizes rapidly. A small amount of the vapor enters the column while the major portion exits from the split/purge vent. The ratio of column flow to split vent flow is controlled by the user. Split injections are primarily used for high concentration samples when you can afford to lose most of the sample out the split/purge vent. It is also used for samples that cannot be diluted. The split ratio is equal to the split vent flow divided by the column flow. If the column has been configured, the desired split ratio can be entered directly. The pneumatics for this inlet in split mode operation are shown in the figure below.
Advanced User Guide
181
Inlets
Split
Carrier Supply 80 PSI
Septum Purge
EPC Module
Frit Valve Valve Valve PS FS PS
Frit
Split Vent Trap
Inlet Weldment
FS = Flow Sensor PS = Pressure Sensor
Column
Split/Splitless inlet splitless mode overview

In this mode, the split vent valve is closed during the injection and remains so while the sample is vaporized in the liner and transferred to the column. At a specified time after injection, the valve opens to sweep any vapors remaining in the liner out the split vent. This avoids solvent tailing due to the large inlet volume and small column flow rate. Specify the purge time and purge flow rate in the inlet parameter list. The septum purge flow may be either on at all times (Standard mode) or on only between the purge time and the end of the run (Switched mode). If you are using gas saver, the gas saver time should be after the purge time.
182
Advanced User Guide
Inlets
Split
Septum Purge
EPC Module
Frit
Split Vent Trap
Inlet Weldment
Column
The S/SL inlet pulsed split and splitless modes

The pressure pulse modes increase inlet pressure just before the beginning of a run and return it to the normal value after a specified amount of time. The pressure pulse: reduces the solvent vapor volume reduces the risk of inlet overload tightens the sample band may allow use of a 2 mm liner, reducing the active glass area If your chromatography is degraded by the pressure pulse, a retention gap may help restore peak shape. You must press [Prep Run] before doing manual injections in the pressure pulse modes. See Pre Run and Prep Run on page 176 for details.
Advanced User Guide
183
Inlets
You can do column pressure and flow programming when in the pressure pulse mode. However, the pressure pulse will take precedence over the column pressure or flow ramp.
Pressure pulse
Pressure or Flow
Pressure or flow program
Split/Splitless inlet split mode minimum operating pressures

The minimum recommended inlet total flow is 20 mL/minute. When the split/splitless inlet is operated in Split mode, there will be a minimum pressure at which the inlet can operate. Typically, low inlet pressures may be required for shorter, wide bore columns. The minimum pressure is a function of carrier gas type, total inlet flow, liner design, and possible contamination of the split vent tube or trap. A wide bore column requires a much lower inlet pressure than a typical capillary column to maintain a given flow. Setting the split ratio (total flow) too high when using a wide bore column can create an unstable control relationship between the pressure and flow control loops.
184
Advanced User Guide
Inlets
Table 28
Approximate minimum viable inlet pressures for split/splitless inlet in split mode, in psi (kPa)
Split vent flow (mL/min) 50100 100200 200400 400600
Helium and hydrogen carrier gases Split liners - 5183-4647, 19251-60540 Splitless liners - 5062-3587, 5181-8818 Nitrogen carrier gas Split liners - 19251-60540, 5183-4647 Splitless liners - 5062-3587, 5181-8818 3.0 (20.7) 4.0 (27.6) 4.0(27.6) 6.0 (41.4) 2.5 (17.2) 4.0 (27.6) 3.5 (24.1 5.5 (37.9) 4.5 (31) 8.0 (55.2) 6.0 (41.4) 11.0 (75.4)
These numbers are based on the resistance to flow of new, clean inlet systems. Sample condensation in the split vent tube or a dirty filter can make these values non- attainable.
Selecting the correct S/SL inlet liner

Split liner
A good liner for split mode operation will offer very little restriction to the split flow path between the bottom of the liner and the inlet gold seal and between the outside of the liner and the inside of the injection port body. The preferred Agilent split liner, part number 5183- 4647, incorporates a glass positioning bead on the bottom to facilitate this. It will also incorporate glass wool or some other source of surface area inside the liner that provides for complete sample vaporization across the boiling point range of the sample. Select an appropriate liner from Table 29. Table 29
Liner
Split mode liners

Description Low Pressure Drop Positioning Bead Volume 870 L Mode Split Fast Injection Split Fast Injection Split Manual Only Split Manual Only Deactivated Yes No No No Part Number 5183-4647 19251-60540 18740-80190 18740-60840
4mm ID, Glass Wool 990 L Empty Pin & Cup Packed Pin & Cup 800 L 800 L
Advanced User Guide
185
Inlets
Splitless liner
The liner volume must contain the solvent vapor. The liner should be deactivated to minimize sample breakdown during the purge delay. Solvent vapor volume can be reduced by using Pulsed Splitless mode. Use the Vapor Volume Calculator to determine vapor volume requirements.
Vapor volume < 300 L Use 2 mm liner (250 L volume), 5181- 8818 or similar. Vapor volume 225 300 L reduce vapor volume. Vapor volume > 300 L
Consider pulsed splitless mode to
Use 4 mm liner, 5062- 3587 or similar.
Vapor volume > 800 L Consider pulsed splitless mode to reduce vapor volume.
For thermally labile or reactive samples, use G1544- 80700 (open top) or G1544- 80730 (top taper) liners. Table 30
Liner
Splitless mode liners

Description Single Taper Glass Wool Single Taper Dual Taper 2 mm Quartz 2 mm Quartz 1.5 mm Volume 900 uL 900 uL 800 uL 250 uL 250 uL 140 uL Mode Splitless Splitless Splitless Splitless Splitless Deactivated Part Number Yes Yes Yes No Yes 5062-3587 5181-3316 5181-3315 18740-80220 5181-8818 18740-80200
No Direct Inject, Purge and Trap, Headspace Splitless Splitless Yes Yes Yes Yes
Single Taper Glass Wool Single Taper 4 mm Single Taper 4 mm Dual Taper
900 uL 900 uL
5062-3587 5181-3316 G1544-80730 G1544-80700
Direct column connect Direct column connect
186
Advanced User Guide
Inlets
Vapor Volume Calculator

Agilent provides a Vapor Volume Calculator to help you determine if a liner is suitable for a method. To use the calculator install the Agilent Instrument utility provided with the GC. The calculator is also provided with the Agilent G4600AA Lab Advisor software.
Setting parameters for the S/SL split mode

Mode
The current operating modesplit Actual and setpoint inlet temperatures
Temperature Pressure
Actual and setpoint inlet pressure
Split ratio The ratio of split vent flow to column flow. Column flow is set at the Column parameter list. This line appears only if your columns in the flow path are defined. Split flow Flow, in mL/min, from the split vent. This line appears only if your columns in the flow path are defined. Total flow This is the total flow into the inlet, which is the sum of the split vent flow, column flow, and septum purge flow. When you change the total flow, the split ratio and split vent flow change while the column flow and pressure remain the same. Septum Purge Flow, in mL/min, through the septum purge line. Recommended range is 1 to 5 mL/min.
If all columns in the flow path are defined

1 Press [Front Inlet] or [Back Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Split. 3 Set the inlet temperature. 4 If you want a specific split ratio, scroll to Split ratio and
enter that number. Split flow will be calculated for you.

5 If you want a specific split flow, scroll to Split flow and
enter that number. Split ratio will be calculated for you.

6 If desired, turn on Gas saver. Set Saver time after the
injection time. Press [Prep Run] (see Pre Run and Prep Run on page 176) before manually injecting the sample.
Advanced User Guide
187
Inlets
If a column in the flow path is not defined

1 Press [Front Inlet] or [Back Inlet]. 2 Set the inlet temperature. 3 Set Total flow into the inlet. It must exceed your intended
Septum Purge flow. Measure the split vent flow using a flow meter.
4 Subtract split vent flow and septum purge flow (see Pre
Run and Prep Run on page 176) from Total flow to get column flow.
5 Calculate the split ratio (split vent flow/column flow).
Adjust as needed.
Selecting parameters for the S/SL splitless mode

A successful splitless injection consists of these steps:
1 Vaporize the sample and solvent in a heated inlet. 2 Use a low flow and low oven temperature to create a
solvent- saturated zone at the head of the column.

3 Use this zone to trap and reconcentrate the sample at the
head of the column.

4 Wait until all, or at least most, of the sample has
transferred to the column. Then discard the remaining vapor in the inletwhich is mostly solventby opening a purge valve. This eliminates the long solvent tail that this vapor would otherwise cause.
5 Raise the oven temperature to release the solvent and
then the sample from the head of the column. Some experimentation is needed to refine the operating conditions. Table 31 provides starting values for the critical parameters. Table 31
Parameter Oven temperature
Splitless mode inlet parameters

Allowed setpoint range Suggested starting value
No cryo, 24 C to 450 C 10 C below solvent CO2 cryo, 60 C to 450 C boiling point N2 cryo, 80 C to 450 C 0 to 999.9 minutes 0 to 999.9 minutes Inlet purge time 2 x Liner volume Column flow
Oven initial time Inlet purge time
188
Advanced User Guide
Inlets
Table 31
Parameter Gas saver time Gas saver flow

Allowed setpoint range 0 to 999.9 minutes 15 to 1000 mL/min Suggested starting value After purge time 15 mL/min greater than maximum column flow
Setting parameters for the S/SL splitless mode

Mode
The current operating modesplitless Below solvent boiling point
Oven temperature Temperature Pressure kPa
Actual and setpoint inlet temperatures
Actual and setpoint inlet pressure in psi, bar, or
Purge time The time, after the beginning of the run, when you want the purge valve to open. This is the time in which the vaporized sample transfers from the liner to the column. Purge flow The flow, in mL/min, from the purge vent, at Purge time. You will not be able to specify this value if any column in the flow path is not defined. Total flow The actual flow to the inlet during a Pre- run (Pre- run light is on and not blinking) and during a run before purge time. You cannot enter a setpoint at these times. At all other times, Total flow will have both setpoint and actual values. Septum Purge line.
Flow, in mL/min, through the septum purge
Septum Purge Flow Mode Standard (septum purge flow is On at all times) or Switched (septum purge flow is Off during injection, turns On at Purge time).
If all columns in the flow path are definedc

1 Press [Front Inlet] or [Back Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Splitless. 3 Set the inlet temperature.
Advanced User Guide
189
Inlets
4 Enter a Purge time and a Purge flow. 5 If desired, turn on Gas saver. Make certain the time is set
after the Purge time.

6 Press [Prep Run] (see Pre Run and Prep Run on
page 176) before manually injecting a sample (this is automatic for Agilent ALS).

1 Press [Front Inlet] or [Back Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Splitless. 3 Set the inlet temperature. 4 Enter a Purge time. 5 Set your Total flow greater than the sum of column flow
plus the septum purge flowsee Pre Run and Prep Run on page 176to guarantee adequate column flow.
page 176) before manually injecting a sample.
Setting parameters for the S/SL pulsed modes

The pulsed mode parameters are the same as the non- pulsed parameters, but with two additional values.
Pulsed pressure The inlet pressure you want at the start of the run. The pressure rises to this value when [Prep Run] is pressed and remains constant until Pulse time elapses, when it returns to Pressure. Pulse time This is the time after the start of the run when the inlet pressure returns to Pressure.
190
Advanced User Guide
Inlets
About the Multimode Inlet

The Agilent Multimode (MMI) Inlet System has five operating modes: The split mode is generally used for major component analyses. The pulsed split mode is like the split mode, but with a pressure pulse applied to the inlet during sample introduction to speed the transfer of material to the column. The splitless mode is used for trace analyses. The pulsed splitless mode allows for a pressure pulse during sample introduction. The solvent vent mode is used for large volume injection. Either single or multiple injections can be made for each run. The direct mode allows for a direct forward pressure of carrier gas through the column. Both the split vent valve and the septum purge valve are closed. The MMI can be used with both manual and automatic injection. Automatic multiple injections (large volume injections) is not available under GC control alone. See MMI solvent vent mode on page 205.
Septum tightening (MMI)

Septum retainer nuts must be tightened enough to obtain a good gas seal, but not so much as to compress the septum and make it difficult to push a syringe needle through it. For the standard septum retainer nut, an internal spring in the septum retainer applies pressure to the septum. For inlet pressures up to 100 psi, tighten the retainer until the C- ring lifts about 1 mm above the top surface. This is adequate for most situations.
1 mm
Advanced User Guide
191
Inlets
With higher inlet pressures, tighten the septum retainer until the C- ring stops turning, indicating that the retainer is in firm contact with the septum. If using a Merlin Microseal septum, finger tighten the septum nut, until snug (not loose). The pressure capacity depends on the duckbill seal used.
Heating the MMI

Programming the MMI temperature is similar to programming the column oven. Access the inlet parameters by pressing [Front Inlet] or [Back Inlet]. Temperature can be programmed with an initial temperature and up to 10 ramps (rates and plateaus). See MMI split and pulsed split modes on page 195 for details. At the end of the run and during postrun, the MMI is held at its final temperature. This permits backflushing without contaminating the inlet.
Additional temperature ramps

For most purposes, the MMI is designed to hold the sample in the inlet liner until the entire samplethere could be several injectionshas been injected. Then the MMI is heated rapidly to transfer the sample to the column. This can be accomplished with an initial hold, a single ramp, and a hold at the end to complete sample transfer. Additional ramps are available and have several possible uses: The inlet can be heated to a high temperature to thermally clean the liner for the next run. The inlet can be programmed downwardjust set the Final temp below the previous temperatureto reduce thermal stress on the inlet. Downward programming can be used to prepare the inlet for the next run. This can reduce cycle time for greater sample throughput.
Cooling the MMI

For cryo cooled inlets, cryogen can be used to cool the inlet. Set the Use Cryo temperature equal to or higher than the desired inlet temperature. Note that if you set an inlet temperature below the Use Cryo temperature, cryogen will be
192
Advanced User Guide
Inlets
used to cool the inlet. This may have a negative impact on the chromatographic performance of the oven and cause distorted peaks. When a method ends, the cryo cooling setpoint returns to the initial state of the method, unless you load another method. To conserve cryogenic fluid when the GC is idle, load a method that does not use cryo cooling. The GC supports only one type of coolant at a time. See To configure the MMI, PTV or COC coolant on page 30
MMI split mode minimum operating pressures

The minimum recommended inlet total flow is 20 mL/minute. When the inlet is operated in a Split mode, there will be a minimum pressure at which the inlet can operate. Typically, low inlet pressures may be required for shorter, wide bore columns. The minimum pressure is a function of carrier gas type, total inlet flow, liner design, and possible contamination of the split vent tube or trap. A wide bore column requires a much lower inlet pressure than a typical capillary column to maintain a given flow. Setting the split ratio (total flow) too high when using a wide bore column can create an unstable control relationship between the pressure and flow control loops. Table 32 Approximate minimum viable inlet pressures for MMI in split mode, in psi (kPa)
Split vent flow (mL/min) 50100 Helium and hydrogen carrier gases Split liners - 5183-4647, 19251-60540 Splitless liners - 5062-3587, 5181-8818 Nitrogen carrier gas Split liners - 19251-60540, 5183-4647 Splitless liners - 5062-3587, 5181-8818 3.0 (20.7) 4.0 (27.6) 4.0(27.6) 6.0 (41.4) 2.5 (17.2) 4.0 (27.6) 3.5 (24.1 5.5 (37.9) 4.5 (31) 8.0 (55.2) 6.0 (41.4) 11.0 (75.4) 100200 200400 400600
These numbers are based on the resistance to flow of new, clean inlet systems. Sample condensation in the split vent tube or a dirty filter can make these values non- attainable.
Advanced User Guide
193
Inlets
Selecting the correct MMI liner

Split liner
A good liner for split mode operation will offer very little restriction to the split flow path between the bottom of the liner and the inlet body and between the outside of the liner and the inside of the inlet body. The preferred Agilent split liner, part number 5183- 4647, incorporates a glass positioning bead on the bottom to facilitate this. It will also incorporate glass wool or some other source of surface area inside the liner that provides for complete sample vaporization across the boiling point range of the sample. Select an appropriate liner from Table 33. Table 33
Liner
Split mode liners

Description Low Pressure Drop Positioning Bead Volume 870 L Mode Split Fast Injection Split Fast Injection Split Manual Only Split Manual Only Deactivated Yes No No No Part Number 5183-4647 19251-60540 18740-80190 18740-60840
4mm ID, Glass Wool 990 L Empty Pin & Cup Packed Pin & Cup 800 L 800 L
Splitless liner
The liner volume must contain the solvent vapor. The liner should be deactivated to minimize sample breakdown during the purge delay. Solvent vapor volume can be reduced by using Pulsed Splitless mode. Use the Vapor Volume Calculator to determine vapor volume requirements.
Vapor volume < 300 L Use 2 mm liner (250 L volume), 5181- 8818 or similar. Vapor volume 225 300 L reduce vapor volume. Vapor volume > 300 L
Consider pulsed splitless mode to
Use 4 mm liner, 5062- 3587 or similar.
Vapor volume > 800 L Consider pulsed splitless mode to reduce vapor volume.
194
Advanced User Guide
Inlets
For thermally labile or reactive samples, use G1544- 80700 (open top) or G1544- 80730 (top taper) liners. Table 34
Liner
Splitless mode liners

Description Single Taper Glass Wool Single Taper Dual Taper 2 mm Quartz 2 mm Quartz 1.5 mm Volume 900 uL 900 uL 800 uL 250 uL 250 uL 140 uL Mode Splitless Splitless Splitless Splitless Splitless Deactivated Part Number Yes Yes Yes No Yes 5062-3587 5181-3316 5181-3315 18740-80220 5181-8818 18740-80200
Direct No Inject, Purge and Trap, Headspace Splitless Splitless Yes Yes Yes Yes
Single Taper Glass Wool Single Taper 4 mm Single Taper 4 mm Dual Taper
900 uL 900 uL
5062-3587 5181-3316 G1544-80730 G1544-80700
Direct column connect Direct column connect
Vapor Volume Calculator

Agilent provides a Vapor Volume Calculator to help you determine if a liner is suitable for a method. To use the calculator install the Agilent Instrument utility provided with the GC. The calculator is also provided with the Agilent G4600AA Lab Advisor software.
MMI split and pulsed split modes

The two split modeswith or without a pressure pulsedivide the gas stream entering the inlet between the column flow and the split vent flow through the solenoid valve. The ratio of the split vent flow to the column flow is called the split ratio.
Advanced User Guide
195
Inlets
The next figure shows the flows with split and pulsed split modes.
Split Carrier Supply 80 PSI Septum Purge
EPC Module
Frit Valve Valve Valve
Frit
PS FS PS
Split Vent Trap
MMI Weldment
FS = Flow Sensor
Cold split introduction

For cold split sample introduction, use an initial inlet temperature below the normal boiling point of the solvent. If the liner volume is enough to hold all the vaporized solvent, start the first inlet temperature ramp at 0.1 minutes with a high heating rate (500 C/min or higher). The final temperature should be high enough to volatilize the heaviest analytes from the liner and should be held for at least 5 minutes. A final temperature of 350 C for 5 minutes has proven sufficient to quantitatively transfer C44. For larger injection volumes or to eliminate the solvent, hold the initial temperature long enough to vent the solvent through the split vent and then begin the first ramp. Use a fast rate for thermally stable analytes. Slower rates may help minimize thermal degradation in the inlet.
196
Advanced User Guide
Inlets
A single temperature ramp is enough for the injection process. The remaining ramps may be used to clean the liner or to reduce the inlet temperature in preparation for the next injection.
Hot split introduction

For hot split introduction, set an initial temperature high enough to volatilize the analytes. No additional thermal parameters are required as the inlet will maintain the setpoint throughout the run.
Setting parameters for split mode operation

Mode:
The current operating modesplit or pulsed split Actual and setpoint inlet temperatures. Starting temperature for the inlet.
Temperature
Initial temperature Initial time Rate #
Hold time at the inlet initial temperature.
Temperature program rates for inlet thermal ramps. Final inlet temperature for ramp 1- 10. Hold time at Final temp 1- 10.
Final temp # Final time #
Pressure Actual and setpoint inlet pressure. Controls capillary column flow and linear velocity. Split ratio The ratio of split flow to column flow. Column flow is set in the column parameter list. This line does not appear if a column in the flow path is not defined. Split flow Flow, in mL/min, from the split/purge vent. This line does not appear if a column in the flow path is not defined. Total flow These are the actual and setpoint values of the total flow into the inlet, which is the sum of the split flow, column flow, and septum purge flow. When you change the total flow, the split ratio and split flow change while the column flow and pressure remain the same. Septum Purge Gas saver
Advanced User Guide
Flow through the septum purge vent.
On to reduce split vent flow at Saver time.

197
Inlets
Saver flow Saver time
Reduced split vent flow, at least 15 mL/min. Time when flow is reduced to save gas.

1 Press [Front Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Split or
Pulsed split.
3 Set the inlet temperature (Initial temperature) and any
desired ramps.
4 If you want a specific split ratio, scroll to Split ratio and
enter that number. The split flow will be calculated and set for you.
enter that number. The split ratio will be calculated and displayed for you.
6 If you selected Pulsed split, enter values for Pulsed pressure
(pressure at injection) and Pulse time (minutes after injection to return to normal pressure).
7 If desired, turn on Gas saver. Set the Saver time after the
injection time.
8 Press [Prep Run] before manually injecting the sample if
the Gas Saver is on (see Pre Run and Prep Run on page 176 for details.).

1 Press [Front Inlet]. 2 Set the inlet temperature (Initial temperature) and any
desired ramps.
3 Set other parameters as described for a defined column. 4 Set Total flow into the inlet. Measure flows out of the split
vent and septum purge vent using a flow meter.

5 Subtract the septum purge flow and split vent flow from
Total flow to get column flow.

Adjust as needed
198
Advanced User Guide
Inlets
MMI splitless and pulsed splitless modes

In these modeswith or without a pressure pulsethe split vent valve is closed during injection and vaporization of the sample and stays so while the sample transfers to the column. At a specified time after injection, the valve opens to sweep vapors left in the liner out the split vent. This avoids solvent tailing due to the large inlet volume and small column flow rate.
Stage 1. Sample injection

With the split vent valve closed, the sample and solvent transfer to the column.
Carrier Supply 80 PSI Septum Purge
EPC Module
Frit
Split Vent Trap
MMI Weldment
Column
Advanced User Guide
199
Inlets
Stage 2. Solvent purging

After the sample has transferred to the column, the split vent valve opens to purge remaining solvent vapor from the inlet.
EPC Module
Frit
PS FS PS
Split Vent Trap
MMI Weldment
Column
200
Advanced User Guide
Inlets
Timelines
This figure summarizes the flow, pressure, and temperature changes during a splitless mode analysis.
Split vent flow Purge flow
Inlet is pressure controlled Inlet pressure Prep Run Start Run Purge Time Saver Time Stop Run Post pressure Column mode = Constant flow
Saver flow
Post Time
Inlet pressure
Inlet temperature
Prep Run
Start Run
Purge Time Final temp 1
Stop Run
Post Time
Initial temperature
Prep Run
Start Run
Purge Time
Advanced User Guide
201
Inlets
Cold splitless introduction

For cold splitless introduction, use an initial inlet temperature below the normal boiling point of the solvent. For most solvents, starting the first inlet temperature ramp at 0.1 minutes provides good transfer and reproducibility. A program rate of 500 C/min or higher is appropriate for thermally stable analytes. A final temperature of 350 C, held for 5 minutes, has quantitatively transferred up to C44 alkane. A main advantage of temperature programmability is that the inlet can be heated gently to transfer delicate analytes. If the oven temperature is initially low enough to refocus the analytes on the column, the inlet heating rate can be made slower (e.g., 120 C/min). This reduces thermal degradation from the inlet and can improve peak shape and quantitation. For most applications of cold splitless, a single temperature ramp is enough. The remaining ramps can be used to clean the liner or to decrease the inlet temperature to prepare for the next injection.
Hot splitless introduction

For hot splitless introduction, select an initial temperature high enough to volatilize the analytes. No additional temperature parameters are required as the inlet will maintain the setpoint throughout the run.
Starting values
1 Inject the sample and temperature program the inlet to
vaporize it.
2 Use a low column flow and low oven temperature to
create a solvent- saturated zone at the head of the column.

head of the column.

5 Raise the oven temperature to analyze the sample.
202
Advanced User Guide
Inlets
Some experimentation is needed to refine the operating conditions. Table 35 provides starting values for the critical parameters. Table 35

Allowed setpoint range No cryo, ambient+4 C to 450 C CO2 cryo, 40 C to 450 C N2 cryo, 80 C to 450 C 0 to 999.9 minutes 0 to 200.0 minutes 0 to 999.9 minutes 15 to 200 mL/min Suggested starting value 10 C below solvent boiling point Inlet purge time 2 x Liner volume Column flow After purge time 15 mL/min greater than maximum column flow 10 C below solvent boiling point for 0.1min, then ramp up
Oven initial time Inlet purge time Gas saver time Gas saver flow
Inlet temperature
No cryo, oven temp + 10 C CO2 cryo, 70 C to 450 C N2 cryo, 160 C to 450 C
Setting parameters for the splitless modes

Mode: The current operating modeSplitless or Pulsed splitless. Temperature Initial time Rate #
Actual and setpoint inlet temperatures. Hold time at the initial inlet temperature.
Temperature program rates for inlet thermal ramps. Final inlet temperature for ramp 1- 10. Hold time at Final temp 1- 10.
Final temp # Final time # Pressure kPa
Pulsed pres The inlet pressure you desire at the beginning of a run. The pressure rises to this setpoint after [Prep Run] is pressed and remains constant until Pulse time elapses, when it returns to Pressure.
Advanced User Guide
203
Inlets
Pulse time time.
Pressure returns to its normal setpoint at this
Purge time The time, after the beginning of the run, when you want the split vent valve to open. Purge flow The flow, in mL/min, from the split vent, at Purge time. You will not be able to specify this value if operating with your column not defined. Total flow The Total flow line displays the actual flow to the inlet during a Pre- run (Pre- run light is on and not blinking) and during a run before purge time. You cannot enter a setpoint at these times. At all other times, Total flow will have both setpoint and actual values. Septum purge Gas saver Server flow Server time
Flow through the septum purge vent
On to reduce split vent flow at Saver time Reduced split vent flow, at least 15 mL/min Time when flow is reduced to save gas
If the column is defined

1 Press [Front Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Splitless or
Pulsed splitless.
3 Set the inlet temperature and any desired ramps. 4 Enter a Purge time and a Purge flow. 5 If desired, turn Gas saver on. Make certain the time is set

page 176) before manually injecting a sample. This is automatic if an Agilent sampler is used.
If the column is not defined

Pulsed splitless.
3 Set the inlet temperature and any desired ramps. 4 Enter a Purge flow.
204
Advanced User Guide
Inlets
5 Enter the Purge time when you wish the split valve to
open.
6 Set Total flow greater than the column flow plus the
septum purge flow to guarantee adequate column flow.

7 Turn Gas saver on, if desired. Set the time after Purge time. 8 Press [Prep Run] (see Pre Run and Prep Run on
MMI solvent vent mode

This mode is typically used for large volume injections. For single injection use a 50 to 500 L syringe and the ALS variable plunger speed to slowly inject the sample. The sample is injected into a cold inlet. If conditions are properly chosen and the sample is suitable, analytes deposit in the inlet liner while the solvent evaporates and is swept out. Large or multiple injections can be used to concentrate sample in the inlet before transferring to the column for analysis.
Stage 1. Sample and vent

During sampling and venting, the split valve is open. The inlet is at Initial temperature, which is at or below the solvent boiling point. Solvent vapors are swept out the vent, while sample deposits on the liner walls or packing.
Advanced User Guide
205
Inlets
Split
Septum Purge
EPC Module
Frit
PS FS PS
Split Vent Trap
MMI Weldment
Column
Stage 2.
Sample transfer
When solvent venting ends, the split valve vent closes and the inlet heats to Final temperature 1. The sample transfers to the capillary column during Purge time. (Purge flow to split vent in a data system).
206
Advanced User Guide
Inlets
Septum Purge
EPC Module
Frit
Split Vent Trap
MMI Weldment
Column
Stage 3. Purge and cleanup

The split valve opens again and the system returns to the Stage 1 configuration but with different setpoints. The MMI is flushed. Additional ramp rates are available to thermally clean the inlet or to reduce inlet temperature after sample transfer. This can extend the life of the liner.
Temperature, pressure, and flow considerations

The solvent vent mode goes through three distinct pneumatic states; venting, sample transfer, and purging. The vent portion allows the inlet pressure and the vent flow to be adjusted to optimize solvent elimination. The transfer state mimics traditional splitless operation and transports the analytes from the liner to the column. The purging mode allows the user to prepare the inlet for the next run.
Advanced User Guide
207
Inlets
A fundamental difficulty with solvent vent mode is the potential loss of volatile analytes with the solvent. Several solutions are possible for this situation: The inlet liner can be packed with a more retentive material, such as Tenax. This greatly improves volatile analyte recovery but may impact recovery of higher boiling materials. Some of the solvent can be left in the liner when sample transfer begins. The residual solvent acts like a stationary phase and retains volatile material, but at the expense of a larger solvent peak. The inlet temperature can be reduced. This reduces the vapor pressure of the volatile analytes and permits higher recoveries. Solvent removal can be speeded up by: Reducing pressure in the inlet during sample introductionthe Vent pressure parameter Increasing flow through the inletthe Vent flow parameter While all these possibilities do complicate use of the PTV, they provide increased flexibility and new potential to solve difficult problems.
Sequence of operations
These are the steps in a typical analysis using the solvent vent mode: Table 36
Step 1 Before injection
The solvent vent process

Parameter Flow at split vent Inlet pressure Value Either Purge flow or Saver flow Derived from column setpoint
The system is resting, with Purge flow (or Saver flow, if on) through the inlet. 2 Prep Run begins Flow at split vent Inlet pressure Vent flow setpoint Vent pressure setpoint
Setpoints change to prepare for injection. When GC is ready, the sample is injected. Inlet and oven temperature program Init times begin. Solvent venting and analyte trapping begin. 3 At Vent end time Flow at split vent Inlet pressure Solvent venting ends, analyte transfer begins as inlet heats up. None, split valve closed Column pressure setpoint
208
Advanced User Guide
Inlets
Table 36
Step 4
The solvent vent process (continued)

Parameter At Purge time Flow at split vent Inlet pressure Value Purge flow setpoint Column pressure setpoint
Analyte transfer ends, inlet is purged of residual vapor. Analysis begins. 5 At Saver time Flow at split vent Inlet pressure Analysis ends, carrier flow reduced to save gas (if Saver is on). Saver flow setpoint Column pressure setpoint
Some important points

The flow through the column is governed by the pressure in the inlet. This is controlled, during the analysis part of the process, by the flow or pressure setpoint or program entered for the column. The controlling times must be in the order shown; Vent end time before Purge time, and Purge time before Saver time. Vent end time must occur before the inlet starts to heat and release analytes. Purge time must occur before the oven begins to heat and move sample through the column.
Timelines
Time increases downward; all other quantities increase to the right.
Advanced User Guide
209
Inlets
Time
Between runs Prep Run Start Run
Oven temperature
Inlet temperature
Inlet pressure
Controlled by column flow or pressure setpoint or program
Split vent flow

Saver or Purge flow
Vent pressure Initial time
Vent flow
Vent end time Rate 1 Initial time Final temperature 1 Final time 1 Purge time Controlled by column flow or pressure setpoint or program Inlet is pressure controlled
Rate 1
Other rates, temperatures, and times, if desired
Purge flow
Final temperature 1 Final time 1 Saver time Other rates, temperatures, and times, if desired Saver flow, if on
When is Start Run?

Both the inlet and oven temperature programs begin at Start Run. All timessuch as Purge timeare measured from Start Run. When does Start Run occur? If the sample is injected manually, Start Run occurs when the user presses the [Start] key. If a single injection per run is made using an autosampler, Start Run occurs when the syringe carrier moves down to make the injection. If multiple injections per run are made using an autosampler, Start Run occurs when the syringe carrier moves down to make the first injection of the set. There are no Start Run signals for the rest of the injections in the set.
210
Advanced User Guide
Inlets
These additional injections take time. The inlet and oven temperature programs, mainly the Initial time values, must be adjusted to allow for this. So must the various time values that control the inlet operation. This is discussed in more detail under To develop a MMI method that uses large volume injection on page 214.
Setting parameters for solvent vent operation

Mode:
The current operating modesolvent vent. Actual and setpoint initial inlet temperatures.
Temperature
Initial time The time, measured from Start Run, when the initial inlet temperature hold ends. Must be greater than Vent end time. Rate #
Temperature program rate for inlet thermal ramps. Final inlet temperature for ramp 1- 10.
Final temperature #
Final time # Hold time at Final temp #. This time is a duration; it is not measured from Start Run. Pressure Actual and setpoint inlet pressure before and after the vent period. It sets the starting point of column head pressure. Vent pressure The inlet pressure during the vent period. By decreasing the inlet pressure while venting, solvent elimination proceeds faster. Also, the pressure reduction decreases the amount of carrier gasand solvent vaporthat enters the column during this time.
Users select from 0 to 100 psig. If 0 is chosen, the inlet uses the lowest pressure possible at the given vent flow. Table 37 shows approximate values for this minimum at various vent flows of helium. Pressures less than those in the table are not possible unless the flow is reduced. Table 37 Minimum attainable pressures
Actual vent pressure at 0 psig setpoint 0.7 1.3 Actual vent pressure at 0 kPa setpoint 5 10
Vent flow (mL/min) 50 100
Advanced User Guide
211
Inlets
Table 37
Minimum attainable pressures

Actual vent pressure at 0 psig setpoint 2.6 6.4 12.7 Actual vent pressure at 0 kPa setpoint 18 44 88
Vent flow (mL/min) 200 500 1000
Vent flow The flow of carrier gas out the split vent during the vent period. Higher flows sweep the liner more quickly and reduce the time for solvent elimination. For most columns, 100 mL/min vent flow eliminates solvent at an acceptable rate but puts minimal material on the column. Vent end time The time, measured from Start Run, when solvent venting ends. For large volume injections, this time is normally greater than the time for the injection to complete. Purge time The time, measured from Start Run, when sample transfer ends. It began at Vent end time. Purge flow The flow of carrier gas to the inlet beginning at Purge time. Total flow
The actual flow into the inlet. Flow through the septum purge vent
Septum Purge Gas saver Saver flow Saver time

1 Press [Front Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Solvent vent. 3 Enter a Vent pressure, a Vent flow, and a Vent end time. 4 Set the inlet temperature and ramps, as desired. 5 Enter a Purge time and a Purge flow. 6 If desired, turn Gas saver on. Make certain the time is set
212
Advanced User Guide
Inlets

1 Set up the parameters as described for the defined
column case.
2 Set Total flow greater than the column flow plus the septum
purge flow to guarantee adequate column flow.
MMI Direct Mode

MMI Direct Mode is a pneumatic configuration that allows on- column like behavior. In this mode, you still use a liner to trap involatile material but the sample can only enter the column. Direct mode works best with direct connect liners. These liners form a seal with the column so that the sample cannot leak out of the liner. The inlet is held at a temperature below the solvent boiling point, just as in cool on- column (COC) during the injection. Pneumatically, the inlet is in forward pressure regulation, similar to the splitless portion of splitless mode. The inlet is then temperature programmed to transfer any remaining volatile material to the column. The only control parameter for Direct Mode is inlet pressure. You can run the column in any of its normal control modes (constant pressure, constant flow, ramped pressure, ramped flow). Gas saver does not work in this mode as there is no purge state. The next figure shows the flows with direct mode.
Advanced User Guide
213
Inlets
Split
Septum Purge
EPC Module
Frit
Split Vent Trap
MMI Weldment
Column
To develop a MMI method that uses large volume injection

This topic provides a recommended way to change from a splitless injection using a split/splitless inlet to a solvent vent mode injection using a Multimode inlet (MMI). It applies mainly to large volume injections (LVI) using a Multimode inlet, but the concepts can apply to general MMI use. This topic does not consider all items that can impact an analysis, for example the liner, solvent, analyte boiling points, or polarity. This topic also assumes knowledge of your data systemwhen to save a method, how to start a run, how to set up a single run, etc.
214
Advanced User Guide
Inlets
The main advantage of the MMI's solvent vent mode is that you can inject slowly into the inlet, allowing large amounts of solvent to evaporate in the liner (not in the split vent line), concentrating the analytes prior to injection. This requires an injector with variable speed injections, a "large" syringe, and knowledge of the sample and the solvent. When developing a solvent vent method, the goal for the injection is to determine the injection rates and temperatures needed to evaporate the solvent at the rate it enters the inlet. The development technique is to gradually scale up to an injection amount that produces a useful response. The most significant parameters are:
Inlet temperature. Hold the inlet temperature at or slightly below the solvent boiling point until after all the sample has been injected. This is important so that you do not boil away more volatile analytes, or boil away the solvent in the needle and trap your analytes there. An additional point to consider is that the boiling point of the earliest eluting analyte should be 100 C > the boiling point of the solvent. Injection speed. Estimate the evaporation rate of solvent exiting the needle based on solvent type, inlet temperature, vent flow, and pressure. Start with about half that number. Note that you have to make sure that you configure the syringe properly. If not, you will over- or under- load the inlet. Vent time. Make sure the vent time setpoint is greater than the time the needle spends in the inlet. If the vent time is too short, you will overload and contaminate the column and inlet. Change the vent time as you upscale the method.
If using a MMI with an MSD, another tip for method development is to scan for solvent ions. Detecting the solvent ions can be useful in troubleshooting residual solvent bleed onto the column. To develop a MMI method for large volume injection, try the following:
1 Determine a small injection volume that works on a
split/splitless inlet in splitless mode. Choose a volume that does not currently overload the inlet.
2 Start with a 510 uL syringe and make sure the syringe
is properly configured in the instrument and data system.

3 Make sure the column is configured.
Advanced User Guide
215
Inlets
4 Set up the inlet to perform a 1 uL injection. Use the
split/splitless inlet method conditions, except: Start with the inlet temperature cold, near but slightly below the solvent boiling point. For example, if using methylene chloride (boiling point 39 C), start with a temperature of 3039 C. Use Splitless mode. Ramp to the normal split/splitless inlet temperature
5 Note the response achieved. 6 Next, change the inlet mode to Solvent Vent. 7 Check the injector timings. a Install an empty sample vial in the injector turret or
tray.
b Input the injection rate (Draw, Dispense, and Inject
rates) for the injector and increase the injection volume to 5 uL.
c Enter draft Solvent Vent parameters:
Set a Vent Flow of 100 mL/min as a starting point. Keep the inlet isothermal for now Enter a Vent Pressure of 0 psi (0 kPa) until 0.1 min. Make an injection using the empty vial. Use a stopwatch or your GC's timer feature to time how long the needle is in the inlet.
8 Enter revised Solvent Vent mode parameters.
Set the method's Vent Time to be about 0.05 min longer than the time the needle spends in the inlet. Set the inlet temperature initial Hold Time to be about 0.05 min longer than the vent pressure until time. Program the inlet to ramp quickly to the injection temperature. Make sure the ramp starts after the vent pressure until time. Set the Purge Flow to Split Vent to 30 mL/min. Set the purge time to be the vent pressure until time + 1 minute.
9 Make a 5 uL injection of your standard. You should see 5
times the response. If the response of all analytes is too low: The dispense speed is too fast. Liquid was injected into the inlet and pushed out the vent.
216
Advanced User Guide
Inlets
The vent time is too long. The inlet started to heat while the vent was open. If the response of early eluters is too low: The inlet temperature is too high. The Vent Flow is too high. If the response of late eluters is too low: The purge time is too short. The final inlet temperature is too low.
10 If you need more injection volume and the 5 uL worked
to give 5X response, change the syringe to a larger one, for example 50 uL.
11 Set up the data system to perform a 25 uL injection. 12 Configure the syringe. Make sure the plunger speeds on
the injector are still set properly.

13 Recheck the injector timings. See step 12. 14 Set a new vent time and initial inlet temperature time
based on the new time the needle spends in the syringe.

15 Make a 25 uL injection of your standard. Again, you
should see 5 times the response. If not, see step 13.

16 If you need more response, repeat steps 10 15 to
increase to larger volume. Also try performing 5 x 5 uL injections, then 5 x 50 uL injections.
Multiple injections with the MMI

The preferred technique for concentrating analytes in the inlet liner is to use a single, large volume injection. Using a high capacity syringe and one septum puncture reduces the possibility of contamination and generally improves results when compared against a multiple septum puncture technique. However, if needed, you can perform multiple septum punctures during the vent time. This technique requires an Agilent data system and automatic liquid sampler.
Data system requirements

An Agilent data system is necessary for multiple injection because the needed parameters are not available through the GC keyboard.
GC ChemStation
Software revision B.04.01 SP1 or later.
Advanced User Guide
217
Inlets
MSD ChemStation EZChrom
Software revision E.02.00 SP2 or later
Software revision 3.3.2 or later
Setting parameters for the inlet in solvent vent mode

Set or configure the following parameters in the data system's 7890A GC method editor. Syringe size Verify the syringe size is configured correctly. The configured syringe size changes the available choices for injection volume. Injection volume Select the injection volume, then enter a number of injections. The total injection volume will be displayed. Multiple Injection Delay A pause time, in seconds, between injections. This is added to the minimum hardware cycle time. Preinjection washes and pumps are performed only before the first injection of a multiple injection set. Postinjection washes are performed only after the last injection in a multiple injection set.
An example
These values were used for a sample with a broad range of boiling points. Table 38
Name Sample Mode MMI liner Injection volume Injection speed Column Column flow
General parameters
Value C10 to C44 hydrocarbons in hexane Solvent vent Glass wool packed One 10.0 L injection (25 L syringe) Fast 30 m x 320 m x 0.25 m -5, part number 19091J-413 4 mL/min constant flow
218
Advanced User Guide
Inlets
Table 39
Name Initial temp Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Final time 2
Inlet parameters
Value 40 C 0.3 min 720 C/min 450 C 5 min 100 C/min 250 C 0 min Name Rate 2 (off) Pressure Vent pressure Vent flow Vent end time Purge time Purge flow 15.6 psig 0.0 psig 100 mL/min 0.2 min 2.0 min 50 mL/min Value
Table 40
Name Initial temp Initial time Rate 1 Final temp 1 Final time 1 Rate 2 (off)
Oven parameters
Value 40 C 2.5 min 25 C/min 320 C 10.0 min
Table 41
Name Detector Detector temp Hydrogen flow Air flow Makeup (N2)
Detector parameters
Value FID 400 C 40 mL/min 450 mL/min 45 mL/min
Advanced User Guide
219
Inlets
C20
These results were compared with a splitless analysis of the same sample, which should produce 100% recovery of all analytes. The data showed that, under these conditions, compounds above C20 were completely recovered and that the recovery was independent of injection size. Compounds lower than C20 were partially vented with the solvent.
Possible adjustments
Depending on what you are trying to accomplish, you have a number of possible adjustments available. To eliminate more solvent Increase the vent end time, inlet initial time, and purge time. This will not affect analytes that are quantitatively trapped but will eliminate more of the solvent peak. Increase the vent flow to sweep the liner more rapidly with the same inlet timing. Increasing vent flow raises vent pressure if it is set to 0. This puts more solvent onto the column.
220
Advanced User Guide
Inlets
Raise the inlet initial temperature to vaporize more solvent and allow more to be eliminated. This also increases the loss of volatile analytes since their vapor pressures also increase. To improve recovery of low boiling analytes Reduce inlet temperature to lower the vapor pressure of the analytes and trap them more effectively. This also reduces solvent vapor pressure and more time will be needed to eliminate it. Use a retentive packing in the liner. Materials such as Tenax permit higher recovery of volatile analytes but may not release higher boiling compounds. This must be considered if quantitation on these high boiling peaks is desired. Leave more solvent in the liner. The solvent acts as a pseudo stationary phase and helps retain volatile analytes. This must be balanced against the detectors tolerance for solvent.
An examplecontinued
The single injection example shown on the last few pages makes it clear that a 10 L injection does not overload the glass wool packed liner. This means that multiple 10 L injections are possible. It was decided to make 10 injections per run, each of 10 L size. This would increase analytical sensitivity substantially. No adjustments were made to improve recovery of the low boilers since the purpose of this analysis was to detect and measure the high boiling components. After timing a trial set of 10 injections, the total time for the multiple injection set was measured to be approximately 1.3 minutes. The following timing changes were made: Table 42
Parameter Inlet Init time Vent end time Purge time Oven Init time
Modifications
Increased from 0.3 minutes 0.2 minutes 2.0 minutes 2.5 minutes To 1.6 minutes 1.5 minutes 3.0 minutes 3.0 minutes
Advanced User Guide
221
Inlets
The result is shown in the next figure. Note the difference in the vertical scale (5000 versus 500).
C20
222
Advanced User Guide
Inlets
About the Packed Column Inlet

This inlet is also known as the purged packed inlet (PP). It is used with packed columns when high- efficiency separations are not required. It can also be used with wide- bore capillary columns, if flows greater than 10 mL/min are acceptable. If the columns are not defined (packed columns and undefined capillary columns), the inlet is usually flow- controlled. If capillary columns are used and the columns in the flow path are defined, the inlet is normally pressure- controlled but can be put into the flow control mode. The figure shows the inlet in the capillary column mode, with the column defined and the flow controlled by pressure.
Advanced User Guide
223
Inlets
Septum Purge
EPC Module Frit Valve Valve FS PS PS Frit
Inlet Weldment
Column
The next figure shows the flow diagram for the packed column mode, with the column not defined the control is based on total carrier gas flow.
224
Advanced User Guide
Inlets
Septum Purge
Inlet Weldment
Packed Column
Setting parameters
The inlet can operate in flow or pressure control mode. Flow is recommended for packed columns. Pressure is recommended for capillary columns.
Inlet in flow control mode

While in flow control mode, you cannot enter pressures here.
Mode Press [Mode/Type] to see the choices. You may select an inlet mode of either Pressure control or Flow control. When the Inlet control mode is Pressure control, the column control mode can be set to Constant pressure, Ramped pressure, Constant
Advanced User Guide
225
Inlets
flow, or Ramped flow. The column control mode is set from the Column parameters display. When the Inlet control mode is Flow control, only column flow can be set on the Column parameters display.
Temperature
The setpoint and actual temperature values.
Pressure The actual pressure (in psi, bar, or kPa) supplied to the inlet. You cannot enter a setpoint here. Total flow Enter your setpoint here, actual value is displayed. Inlet is mass flow controlled. Septum purge The setpoint and actual flow, in mL/min, through the septum purge line, typically 1 to 5 mL/min
Inlet in pressure control mode

While in pressure control mode, you cannot enter flows here.
Mode Press [Mode/Type] to see the choices. You may select an inlet mode of either Pressure control or Flow control. When the Inlet control mode is Pressure control, the column control mode can be set to Constant pressure, Ramped pressure, Constant flow, or Ramped flow. The column control mode is set from the Column parameters display. When the Inlet control mode is Flow control, only column flow can be set on the Column parameters display. Temperature the inlet.
The setpoint and actual temperature values of
Pressure Enter your setpoint here (in psi, bar, or kPa). The actual value is displayed. Total flow The actual total flow to the inlet. This is a reported value, not a setpoint. Septum purge The setpoint and actual flow, in mL/min, through the septum purge line, typically 1 to 5 mL/min
226
Advanced User Guide
Inlets
About the Packed Column Inlet

This inlet is also known as the purged packed inlet (PP). It is used with packed columns when high- efficiency separations are not required. It can also be used with wide- bore capillary columns, if flows greater than 10 mL/min are acceptable. If the columns are not defined (packed columns and undefined capillary columns), the inlet is usually flow- controlled. If capillary columns are used and the columns in the flow path are defined, the inlet is normally pressure- controlled but can be put into the flow control mode. The figure shows the inlet in the capillary column mode, with the column defined and the flow controlled by pressure.
Advanced User Guide
227
Inlets
Septum Purge
Inlet Weldment
Column
The next figure shows the flow diagram for the packed column mode, with the column not defined the control is based on total carrier gas flow.
228
Advanced User Guide
Inlets
Septum Purge
Inlet Weldment
Packed Column
Setting parameters
The inlet can operate in flow or pressure control mode. Flow is recommended for packed columns. Pressure is recommended for capillary columns.
Inlet in flow control mode

While in flow control mode, you cannot enter pressures here.
Mode Press [Mode/Type] to see the choices. You may select an inlet mode of either Pressure control or Flow control. When the Inlet control mode is Pressure control, the column control mode can be set to Constant pressure, Ramped pressure, Constant
Advanced User Guide
229
Inlets
flow, or Ramped flow. The column control mode is set from the Column parameters display. When the Inlet control mode is Flow control, only column flow can be set on the Column parameters display.
Temperature
The setpoint and actual temperature values.
Pressure The actual pressure (in psi, bar, or kPa) supplied to the inlet. You cannot enter a setpoint here. Total flow Enter your setpoint here, actual value is displayed. Inlet is mass flow controlled. Septum purge The setpoint and actual flow, in mL/min, through the septum purge line, typically 1 to 5 mL/min
Inlet in pressure control mode

While in pressure control mode, you cannot enter flows here.
Mode Press [Mode/Type] to see the choices. You may select an inlet mode of either Pressure control or Flow control. When the Inlet control mode is Pressure control, the column control mode can be set to Constant pressure, Ramped pressure, Constant flow, or Ramped flow. The column control mode is set from the Column parameters display. When the Inlet control mode is Flow control, only column flow can be set on the Column parameters display. Temperature the inlet.
The setpoint and actual temperature values of
Pressure Enter your setpoint here (in psi, bar, or kPa). The actual value is displayed. Total flow The actual total flow to the inlet. This is a reported value, not a setpoint. Septum purge The setpoint and actual flow, in mL/min, through the septum purge line, typically 1 to 5 mL/min
230
Advanced User Guide
Inlets
About the Cool On-Column Inlet

This inlet introduces liquid sample directly onto a capillary column. To do this, both the inlet and the oven must be cool at injection, either at or below the boiling point of the solvent. Because the sample does not vaporize immediately in the inlet, problems with sample discrimination and sample alteration are minimized. If done properly, cool- on column injection also provides accurate and precise results. You can operate the inlet in track oven mode, where the inlet temperature follows the column oven, or you can program up to three temperature ramps. A cryogenic cooling option, that uses liquid CO2 or N2 from the oven cryogenic system, can reach subambient temperatures.
EPC Module
Frit Valve Valve PS PS
Frit
Septum
Cool on Column Inlet Weldment
Ferrule
Column Adapter Column Nut Column
PS = Pressure Sensor
Column
Advanced User Guide
231
Inlets
Setup modes of the COC inlet

The COC inlet hardware must be set up for one of three usages, depending on the type of injection and column size. 0.25 mm or 0.32 mm automated on- column. Use predrilled septa. 0.53 mm automatic on- column or retention gap 0.2 mm manual To select the correct hardware for a column and injection type, refer to Maintaining Your GC.
Retention gaps
Because the sample is injected directly onto the column, it is strongly suggested that a retention gapor guard columnbe used to protect your column. A retention gap is a deactivated column that is connected between the inlet and the analytical column. If you choose to use one, it is suggested that at least 1 m of retention gap be installed per 1 L of sample injected. Information on ordering retention gaps can be found in the Agilent catalog for consumables and supplies. If you are using a retention gap and are operating with the column defined, the length of the retention gap could affect the calculations for flow and velocity through your column. If your retention gap is the same inside diameter as your column, it is a good idea to add the retention gap and column length before entering the number on the Configure Column parameter list. If the retention gap inside diameter is larger than your column, this step may not be necessary.
COC inlet temperature control

CryoBlast (optional)
CryoBlast shortens the cycle time between runs. If you have a CO2 or N2 cryogenic valve and the CryoBlast feature, you can cool the inlet to 37 C in either the track oven or temperature program modes. The CryoBlast accessory uses coolant from the oven cryogenic system.
232
Advanced User Guide
Inlets
Track oven mode

In the Track oven mode, the inlet temperature stays 3 C higher than the oven temperature throughout the oven program. You cannot enter a temperature setpointit is set automatically. If you have CryoBlast, the inlet will track oven temperatures to 40C; without CryoBlast, the lower limit is set by room temperature.
Temperature programming mode

In this mode, you can enter up to three temperature ramps in the inlet parameter list so that the inlet and the oven operate independently. This is the recommended mode if operating below 20 C. At these very low oven temperatures, the inlet temperature should be at least 20 C higher than the oven temperature. This will be more than adequate for solvent focusing. At temperatures greater than ambient, the inlet should always be at least 3 C warmer than the oven for proper control of the inlet temperature. The oven temperature program controls the run. If it is longer than the inlet temperature program, the inlet will remain at its final temperature until the oven program (and the run) ends.
Cryogenic considerations
When using track oven mode with a cryogenic oven, all other inlets must be off or in track oven mode.
Setting COC inlet flows/pressures

1 Configure capillary column to inletselect constant flow
or pressure.
2 Set column flow, linear velocity, or inlet pressure. 3 Set Septum Purge, typically 3 to 10 mL/min.
Setting COC inlet parameters

Track oven mode
1 Press [Front Inlet] or [Back Inlet]. 2 Press [Mode/Type] and select Track oven.
Advanced User Guide
233
Inlets
There is no setpoint for Track oven mode.
Ramped temperature mode

1 Press [Front Inlet] or [Back Inlet]. 2 Press [Mode/Type] and select Ramped temp. 3 Enter a value for Temp. This is the starting temperature. 4 Enter an Init time. This is the length of time the inlet will
stay at the starting temperature after a run has begun.

5 Enter Rate 1. This is the rate at which the inlet will be
heated or cooled. A Rate of 0 halts further programming.

6 Enter Final temp 1. This is the inlet temperature at the end
of the first ramp.

7 Enter Final time 1. This is the number of minutes the inlet
holds Final temp 1.

8 To enter a second (or third) ramp, scroll to the
appropriate Rate line and repeat steps 5 through 7.
234
Advanced User Guide
Inlets
About the PTV Inlet

The Agilent Programmed Temperature Vaporization (PTV) Inlet System has five operating modes: The split mode is generally used for major component analyses. The pulsed split mode is like the split mode, but with a pressure pulse applied to the inlet during sample introduction to speed the transfer of material to the column. The splitless mode is used for trace analyses. The pulsed splitless mode allows for a pressure pulse during sample introduction. The solvent vent mode is used for large volume injection. Either single or multiple injections can be made for each run. The PTV inlet can be used with both manual and automatic injection. For automatic multiple injections (large volume injections), an Agilent GC or MSD ChemStation is required. This function is not available under GC control alone. See PTV inlet solvent vent mode on page 248.
PTV sampling heads

Two heads are available for the PTV inlet. The septum head uses either a regular septum or a Merlin Microseal to seal the syringe passage. A stream of gas sweeps the inner side of the septum and exits through the septum purge vent on the pneumatics module. It may be used with either automatic or manual injection. The septum head uses either standard 11 mm septa or (with a different cap) a Merlin Microseal. The septumless head uses a check valve instead of a septum to seal the syringe entrance passage. It may be used with either automatic or manual injection. This head is recommended for subambient inlet operation.
Advanced User Guide
235
Inlets
Septum head
Septumless head
The flow diagrams in the rest of this document show the septum head in place with a separate drawing for the septumless head.
Heating the PTV inlet

The control parameters for PTV temperature programming are the same as for the column oven, but are reached by pressing [Front Inlet]. Temperature can be programmed with an initial temperature and up to 3 rates and plateaus. Rates between 0.1 and 720 C/min can be selected. See Setting COC inlet parameters on page 233 for details. At the end of the run and during postrun, the PTV is held at its final temperature. This permits backflushing without contaminating the inlet.
CAUTION
If the initial inlet temperature and the oven initial temperature are too close, the inlet may be unable to maintain its setpoint. We recommend a difference of at least 6 C, either higher or lower.
Additional temperature ramps

For most purposes, the PTV is designed to hold the sample in the inlet liner until the entire samplethere could be several injectionshas been injected. Then the PTV is heated rapidly to transfer the sample to the column. This can be accomplished with an initial hold, a single ramp, and a hold at the end to complete sample transfer. Two additional ramps are available and have several possible uses: The inlet can be heated to a high temperature to thermally clean the liner for the next run.
236
Advanced User Guide
Inlets
The inlet can be programmed downwardjust set the Final temp below the previous temperatureto reduce thermal stress on the inlet. Downward programming can be used to prepare the inlet for the next run. This can reduce cycle time for greater sample throughput.
Cooling the PTV inlet

The sample may be injected into either a cooled or heated inlet. The initial inlet temperature can be reduced to 60 C (with CO2 cooling) or to 160 C (with liquid N2 cooling). The GC supports only one type of coolant at a time. Once a coolant is selected for any cryogenic device, that same coolant must be used for all such devices, including the column oven. Since the GC can sense which coolant is used by the oven, if oven cooling is installed that coolant becomes the one that must be used by all other cooling devices.
PTV inlet split and pulsed split modes

The two split modeswith or without a pressure pulsedivide the gas stream entering the inlet between the column flow, the split vent flow through the solenoid valve, and the septum purge flow. The ratio of the split vent flow to the column flow is called the split ratio. The next figure shows the flows with the septum head. Flows with the septumless head are the same except that the septum purge flow bypasses the head.
Advanced User Guide
237
Inlets
Split
Septum Purge
EPC Module
Frit
PS FS PS
Split Vent Trap
PTV Inlet Weldment
Column
Cold split introduction

For cold split sample introduction, use an initial inlet temperature below the normal boiling point of the solvent. If the liner volume is enough to hold all the vaporized solvent, start the first inlet temperature ramp at 0.1 minutes with a high heating rate (500 C/min or higher). The final temperature should be high enough to volatilize the heaviest analytes from the liner and should be held for at least 5 minutes. A final temperature of 350 C for 5 minutes has proven sufficient to quantitatively transfer C44. For larger injection volumes or to eliminate the solvent, hold the initial temperature long enough to vent the solvent through the split vent and then begin the first ramp. Use a fast rate for thermally stable analytes. Slower rates may help minimize thermal degradation in the inlet.
238
Advanced User Guide
Inlets
A single temperature ramp is enough for the injection process. The remaining ramps may be used to clean the liner or to reduce the inlet temperature in preparation for the next injection.
Hot split introduction

For hot split introduction, set an initial temperature high enough to volatilize the analytes. No additional thermal parameters are required as the inlet will maintain the setpoint throughout the run. Because of the small liner volume (about 120 microliters), the PTV has a limited injection capacity with hot split introduction. Injection volumes exceeding 1 L in the hot split mode may overflow the inlet causing analytical problems. Cold split introduction avoids this potential problem.
Setting parameters for split mode operation

Mode:
The current operating modesplit or pulsed split Actual and setpoint inlet temperatures. Starting temperature for the inlet.
Temperature
Initial temperature Initial time Rate #
Hold time at the inlet initial temperature.
Temperature program rates for inlet thermal ramps. Final inlet temperature for ramps 1, 2, and 3. Hold time at Final temp 1, 2, and 3.
Final temp # Final time #
Pressure Actual and setpoint inlet pressure. Controls capillary column flow and linear velocity. Split ratio The ratio of split flow to column flow. Column flow is set in the column parameter list. This line does not appear if a column in the flow path is not defined. Split flow Flow, in mL/min, from the split/purge vent. This line does not appear if a column in the flow path is not defined.
Advanced User Guide
239
Inlets
Total flow These are the actual and setpoint values of the total flow into the inlet, which is the sum of the split flow, column flow, and septum purge flow. When you change the total flow, the split ratio and split flow change while the column flow and pressure remain the same. Septum Purge Gas saver Saver flow Saver time
Flow through the septum purge vent.
On to reduce split vent flow at Saver time. Reduced split vent flow, at least 15 mL/min. Time when flow is reduced to save gas.

1 Press [Front Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Split or
Pulsed split.
3 Set the inlet temperature (Initial temperature) and any
desired ramps.
4 If you want a specific split ratio, scroll to Split ratio and
enter that number. The split ratio will be calculated and displayed for you.
6 If you selected Pulsed split, enter values for Pulsed pressure
(pressure at injection) and Pulse time (minutes after injection to return to normal pressure).
7 If desired, turn on Gas saver. Set the Saver time after the
injection time.
8 Press [Prep Run] before manually injecting the sample if
the Gas Saver is on (see Pre Run and Prep Run on page 176).

1 Press [Front Inlet]. 2 Set the inlet temperature (Initial temperature) and any
desired ramps.
3 Set other parameters as described for a defined column. 4 Set Total flow into the inlet. Measure flows out of the split
vent and septum purge vent using a flow meter.
240
Advanced User Guide
Inlets
5 Subtract the septum purge flow and split vent flow from
Total flow to get column flow.

Adjust as needed
PTV inlet splitless and pulsed splitless modes

In these modeswith or without a pressure pulsethe split vent valve is closed during injection and vaporization of the sample and stays so while the sample transfers to the column. At a specified time after injection, the valve opens to sweep vapors left in the liner out the split vent. This avoids solvent tailing due to the large inlet volume and small column flow rate. The figures show the flows with the septum head. Flows with the septumless head are the same except that the septum purge flow bypasses the head.
Stage 1. Sample injection

With the split vent valve closed, the sample and solvent transfer to the column.
Advanced User Guide
241
Inlets
Split
Septum Purge
EPC Module
Frit
Split Vent Trap
PTV Inlet Weldment
Column
Stage 2. Solvent purging

After the sample has transferred to the column, the split vent valve opens to purge remaining solvent vapor from the inlet.
242
Advanced User Guide
Inlets
Split
Septum Purge
EPC Module
Frit
PS FS PS
Split Vent Trap
PTV Inlet Weldment
Column
Timelines
This figure summarizes the flow, pressure, and temperature changes during a splitless mode analysis.
Advanced User Guide
243
Inlets
Split vent flow
Purge flow
Inlet is pressure controlled Inlet pressure Prep Run Start Run Purge Time Saver Time Stop Run Post pressure Column mode = Constant flow
Saver flow
Post Time
Inlet pressure
Inlet temperature
Prep Run
Start Run
Purge Time Final temp 1
Stop Run
Post Time
Initial temperature
Prep Run
Start Run
Purge Time
Cold splitless introduction

For cold splitless introduction, use an initial inlet temperature below the normal boiling point of the solvent. For most solvents, starting the first inlet temperature ramp at 0.1 minutes provides good transfer and reproducibility. A program rate of 500 C/min or higher is appropriate for thermally stable analytes. A final temperature of 350 C, held for 5 minutes, has quantitatively transferred up to C44 alkane. A main advantage of temperature programmability is that the inlet can be heated gently to transfer delicate analytes. If the oven temperature is initially low enough to refocus the analytes on the column, the inlet heating rate can be made slower (e.g., 120 C/min). This reduces thermal degradation from the inlet and can improve peak shape and quantitation.
244
Advanced User Guide
Inlets
For most applications of cold splitless, a single temperature ramp is enough. The remaining ramps can be used to clean the liner or to decrease the inlet temperature to prepare for the next injection.
Hot splitless introduction

For hot splitless introduction, select an initial temperature high enough to volatilize the analytes. No additional temperature parameters are required as the inlet will maintain the setpoint throughout the run. Because of the small liner volume (about 120 L), the PTV cannot contain vapor resulting from large liquid injection volumes. Injection volumes greater than 1 L may overflow vapor from the inlet, causing analysis variations. Cold splitless introduction avoids this problem.
Starting values
1 Inject the sample and temperature program the inlet to
vaporize it.
2 Use a low column flow and low oven temperature to
create a solvent- saturated zone at the head of the column.

head of the column.

5 Raise the oven temperature to analyze the sample.
Some experimentation is needed to refine the operating conditions. Table 43 provides starting values for the critical parameters. Table 43

Allowed setpoint range Suggested starting value
No cryo, ambient+10 C to 450 C 10 C below solvent CO2 cryo, 60 C to 450 C boiling point N2 cryo, 80 C to 450 C 0 to 999.9 minutes Inlet purge time
Oven initial time
Advanced User Guide
245
Inlets
Table 43
Parameter
Splitless mode inlet parameters (continued)

Allowed setpoint range 0 to 999.9 minutes 0 to 999.9 minutes 15 to 1000 mL/min Suggested starting value 2 x Liner volume Column flow After purge time 15 mL/min greater than maximum column flow 10 C below solvent boiling point for 0.1min, then ramp up
Inlet purge time Gas saver time Gas saver flow
Inlet temperature
No cryo, oven temp + 10 C CO2 cryo, 50 C to 450 C N2 cryo, 60 C to 450 C
Setting parameters for the splitless modes

Mode: The current operating modeSplitless or Pulsed splitless. Temperature Initial time Rate #
Actual and setpoint inlet temperatures. Hold time at the initial inlet temperature.
Temperature program rates for inlet thermal ramps. Final inlet temperature for ramps 1, 2, and 3. Hold time at Final temp 1, 2, and 3.
Final temp # Final time # Pressure kPa
Pulsed pres The inlet pressure you desire at the beginning of a run. The pressure rises to this setpoint after [Prep Run] is pressed and remains constant until Pulse time elapses, when it returns to Pressure. Pulse time time.
Pressure returns to its normal setpoint at this
Purge time The time, after the beginning of the run, when you want the split vent valve to open. Purge flow The flow, in mL/min, from the split vent, at Purge time. You will not be able to specify this value if operating with your column not defined.
Inlets
Total flow The Total flow line displays the actual flow to the inlet during a Pre- run (Pre- run light is on and not blinking) and during a run before purge time. You cannot enter a setpoint at these times. At all other times, Total flow will have both setpoint and actual values. Septum purge Gas saver Server flow Server time

Pulsed splitless.
3 Set the inlet temperature and any desired ramps. 4 Enter a Purge time and a Purge flow. 5 If desired, turn Gas saver on. Make certain the time is set


Pulsed splitless.
3 Set the inlet temperature and any desired ramps. 4 Enter a Purge flow. 5 Enter the Purge time when you wish the split valve to
open.
6 Set Total flow greater than the column flow plus the
septum purge flow to guarantee adequate column flow.

7 Turn Gas saver on, if desired. Set the time after Purge time. 8 Press [Prep Run] (see Pre Run and Prep Run on
Advanced User Guide
247
Inlets
PTV inlet solvent vent mode

This mode is typically used for large volume injections. For single injection use a 50 or 100 L syringe with variable plunger speedslowly, 5 to 30 seconds. The sample is injected into a cold inlet. If conditions are properly chosen and the sample is suitable, analytes deposit in the inlet liner while the solvent evaporates and is swept out. Large or multiple injections can be used to concentrate sample in the inlet before transferring to the column for analysis. The figure shows the flows with the septum head. Flows with the septumless head are the same except that the septum purge flow bypasses the head.
Stage 1. Sample and vent

During sampling and venting, the split valve is open. The inlet is at Initial temperature, which is at or below the solvent boiling point. Solvent vapors are swept out the vent, while sample deposits on the liner walls or packing.
248
Advanced User Guide
Inlets
Split
Septum Purge
EPC Module
Frit
PS FS PS
Split Vent Trap
PTV Inlet Weldment
Column
Stage 2.
Sample transfer
When solvent venting ends, the split valve vent closes and the inlet heats to Final temperature 1. The sample transfers to the capillary column during Purge delay time.
Advanced User Guide
249
Inlets
Split
Septum Purge
EPC Module
Frit
Split Vent Trap
PTV Inlet Weldment
Column
Stage 3. Purge and cleanup

The split valve opens again and the system returns to the Stage 1 configuration but with different setpoints. The PTV inlet is flushed. Additional ramp rates are available to thermally clean the inlet or to reduce inlet temperature after sample transfer. This can extend the life of the liner.
Temperature, pressure, and flow considerations

The solvent vent mode goes through three distinct pneumatic states; venting, sample transfer, and purging. The vent portion allows the inlet pressure and the vent flow to be adjusted to optimize solvent elimination. The transfer state mimics traditional splitless operation and transports the analytes from the liner to the column. The purging mode allows the user to prepare the inlet for the next run.
250
Advanced User Guide
Inlets
A fundamental difficulty with solvent vent mode is the potential loss of volatile analytes with the solvent. Several solutions are possible for this situation: The inlet liner can be packed with a more retentive material, such as Tenax. This greatly improves volatile analyte recovery but may impact recovery of higher boiling materials. Some of the solvent can be left in the liner when sample transfer begins. The residual solvent acts like a stationary phase and retains volatile material, but at the expense of a larger solvent peak. The inlet temperature can be reduced. This reduces the vapor pressure of the volatile analytes and permits higher recoveries. Solvent removal can be speeded up by: Reducing pressure in the inlet during sample introductionthe Vent pressure parameter Increasing flow through the inletthe Vent flow parameter While all these possibilities do complicate use of the PTV, they provide increased flexibility and new potential to solve difficult problems.
Sequence of operations
These are the steps in a typical analysis using the solvent vent mode: Table 44
Step 1 Before injection
The solvent vent process

Parameter Flow at split vent Inlet pressure Value Either Purge flow or Saver flow Derived from column setpoint
The system is resting, with Purge flow (or Saver flow, if on) through the inlet. 2 Prep Run begins Flow at split vent Inlet pressure Vent flow setpoint Vent pressure setpoint
Setpoints change to prepare for injection. When GC is ready, the sample is injected. Inlet and oven temperature program Init times begin. Solvent venting and analyte trapping begin. 3 At Vent end time Flow at split vent Inlet pressure Solvent venting ends, analyte transfer begins as inlet heats up. None, split valve closed Column pressure setpoint
Advanced User Guide
251
Inlets
Table 44
Step 4
The solvent vent process (continued)

Parameter At Purge time Flow at split vent Inlet pressure Value Purge flow setpoint Column pressure setpoint
Analyte transfer ends, inlet is purged of residual vapor. Analysis begins. 5 At Saver time Flow at split vent Inlet pressure Analysis ends, carrier flow reduced to save gas (if Saver is on). Saver flow setpoint Column pressure setpoint
Some important points

The flow through the column is governed by the pressure in the inlet. This is controlled, during the analysis part of the process, by the flow or pressure setpoint or program entered for the column. The controlling times must be in the order shown; Vent end time before Purge time and PTV temperature Initial time before Saver time. Vent end time must occur before the inlet starts to heat and release analytes. Purge time must occur before the oven begins to heat and move sample through the column.
Timelines
Time increases downward; all other quantities increase to the right.
252
Advanced User Guide
Inlets
Time
Between runs Prep Run Start Run
Oven temperature
Inlet temperature
Inlet pressure
Controlled by column flow or pressure setpoint or program
Split vent flow

Saver or Purge flow
Vent pressure Initial time
Vent flow
Vent end time Rate 1 Initial time Final temperature 1 Final time 1 Purge time Controlled by column flow or pressure setpoint or program Inlet is pressure controlled
Rate 1
Other rates, temperatures, and times, if desired
Purge flow
Final temperature 1 Final time 1 Saver time Other rates, temperatures, and times, if desired Saver flow, if on
When is Start Run?

Both the inlet and oven temperature programs begin at Start Run. All timessuch as Purge timeare measured from Start Run. When does Start Run occur? If the sample is injected manually, Start Run occurs when the user presses the [Start] key. If a single injection per run is made using an autosampler, Start Run occurs when the syringe carrier moves down to make the injection. If multiple injections per run are made using an autosampler, Start Run occurs when the syringe carrier moves down to make the first injection of the set. There are no Start Run signals for the rest of the injections in the set.
Advanced User Guide
253
Inlets
These additional injections take time. The inlet and oven temperature programs, mainly the Initial time values, must be adjusted to allow for this. So must the various time values that control the inlet operation. This is discussed in more detail under To develop a PTV method that uses large volume injection on page 256.
Setting parameters for solvent vent operation

Mode:
The current operating modesolvent vent. Actual and setpoint initial inlet temperatures.
Temperature
Initial time The time, measured from Start Run, when the initial inlet temperature hold ends. Must be greater than Vent end time. Rate #
Temperature program rate for inlet thermal ramps. Final inlet temperature for ramps 1, 2,
Final temperature # and 3.
Final time # Hold time at Final temp #. This time is a duration; it is not measured from Start Run. Pressure Actual and setpoint inlet pressure before and after the vent period. It sets the starting point of column head pressure. Vent pressure The inlet pressure during the vent period. By decreasing the inlet pressure while venting, solvent elimination proceeds faster. Also, the pressure reduction decreases the amount of carrier gasand solvent vaporthat enters the column during this time.
Users select from 0 to 100 psig. If 0 is chosen, the inlet uses the lowest pressure possible at the given vent flow. Table 45 shows approximate values for this minimum at various vent flows of helium. Pressures less than those in the table are not possible unless the flow is reduced. Table 45 Minimum attainable pressures
Actual vent pressure at 0 psig setpoint 0.7 1.3 Actual vent pressure at 0 kPa setpoint 5 10
Vent flow (mL/min) 50 100
254
Advanced User Guide
Inlets
Table 45
Minimum attainable pressures

Actual vent pressure at 0 psig setpoint 2.6 6.4 12.7 Actual vent pressure at 0 kPa setpoint 18 44 88
Vent flow (mL/min) 200 500 1000
Vent flow The flow of carrier gas out the split vent during the vent period. Higher flows sweep the liner more quickly and reduce the time for solvent elimination. For most columns, 100 mL/min vent flow eliminates solvent at an acceptable rate but puts minimal material on the column. Vent end time The time, measured from Start Run, when solvent venting ends. For large volume injections, this time is normally greater than the time for the injection to complete. Purge time The time, measured from Start Run, when sample transfer ends. It began at Vent end time. Purge flow The flow of carrier gas to the inlet beginning at Purge time. Total flow
The actual flow into the inlet. Flow through the septum purge vent

1 Press [Front Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Solvent vent. 3 Enter a Vent pressure, a Vent flow, and a Vent end time. 4 Set the inlet temperature and ramps, as desired. 5 Enter a Purge time and a Purge flow. 6 If desired, turn Gas saver on. Make certain the time is set
Advanced User Guide
255
Inlets

1 Set up the parameters as described for the defined
column case.
2 Set Total flow greater than the column flow plus the septum
purge flow to guarantee adequate column flow.
To develop a PTV method that uses large volume injection

This topic provides a recommended way to change from a splitless injection using a split/splitless inlet to a solvent vent mode injection using a programmable temperature vaporization inlet (PTV). It applies mainly to large volume injections (LVI) using a PTV, but the concepts can apply to general PTV use. This topic does not consider all items that can impact an analysis, for example the liner, solvent, analyte boiling points, or polarity. This topic also assumes knowledge of your data systemwhen to save a method, how to start a run, how to set up a single run, etc. The main advantage of the PTV inlet's solvent vent mode is that you can inject slowly into the inlet, allowing large amounts of solvent to evaporate in the liner (not in the split vent line). This concentrates the analytes prior to injection. It requires an injector with variable speed injections, a large syringe, and knowledge of the sample and the solvent. When developing a solvent vent method, the goal is to determine the injection rates and temperatures needed to evaporate the solvent at the rate it enters the inlet. The development technique is to gradually scale up to an injection amount that produces a useful response. The most significant parameters are:
Temperature Hold the inlet temperature at or slightly below the solvent boiling point until after all the sample has been injected. This is important so that you do not boil away more volatile analytes, or boil away the solvent in the needle and trap your analytes there. An additional point to consider is that the boiling point of the earliest eluting analyte should be 100 C less than the boiling point of the solvent.
256
Advanced User Guide
Inlets
Injection speed Estimate the evaporation rate of solvent exiting the needle based on solvent type, inlet temperature, vent flow, and pressure. Start with about half that number. Note that you have to make sure that you configure the syringe properly. If not, you will over- or under- load the inlet. Vent end time The vent end time setpoint must be greater than the time the needle spends in the inlet. If the vent time is too short, you will overload and contaminate the column and inlet. Adjust the vent time as you scale up the method.
If using a PTV with an MSD, another tip for method development is to scan for solvent ions. Detecting the solvent ions can be useful in troubleshooting residual solvent bleed onto the column. To develop a PTV method for large volume injection, try the following:
1 Determine a small injection volume that works on a
split/splitless inlet in splitless mode or the PTV in splitless mode. Choose a volume that does not currently overload the inlet.
2 Start with a 510 uL syringe and make sure the syringe
is properly configured in the instrument and data system.

3 Make sure the column is configured. 4 Set up the inlet to perform a 1 uL injection.
Use the splitless method conditions, except: Start with the inlet temperature cold, near but slightly below the solvent boiling point. For example, if using methylene chloride (boiling point 39 C), start with a temperature of 3039 C. Use Splitless mode. Ramp to the normal splitless inlet temperature.
5 Note the response achieved. 6 Next, change the inlet mode to Solvent vent. 7 Check the injector timings. a Install an empty sample vial in the injector turret or
tray.
b Input the injection rate (Sample Draw Speed, Sample Disp
Speed, and Inject Dispense Speed rates) for the injector and increase the injection volume to 5 uL.
c Enter draft Solvent vent parameters:
Advanced User Guide
257
Inlets
Set a Vent flow of 100 mL/min as a starting point. Keep the inlet isothermal for now. Enter a Vent pressure of 0 psi (0 kPa) and Vent end time of 0.1 minutes.
d Make an injection using the empty vial. Use a
stopwatch or your GC's timer feature to time how long the needle is in the inlet.
8 Enter revised Solvent vent mode parameters.
Set the method's Vent end time to be about 0.05 min longer than the time the needle spends in the inlet. Set the inlet temperature Initial time to be about 0.05 min longer than the Vent pressure time. Program the inlet to ramp quickly to the injection temperature. Make sure the ramp starts after the Vent end time. Set the Purge Flow to 30 mL/min. Set the purge time to be the vent pressure Vent end time + 1 minute.
9 Make a 5 uL injection of your standard. You should see 5
times the response. If the response of all analytes is too low: The dispense speed is too fast. Liquid was injected into the inlet and pushed out the vent. The vent time is too long. The inlet started to heat while the vent was open. If the response of early eluters is too low: The inlet temperature is too high. The Vent flow is too high. If the response of late eluters is too low: The purge time is too short. The final inlet temperature is too low.
10 If you need more injection volume and the 5 uL worked
to give 5 times the response, change the syringe to a larger one, for example, 50 uL.
11 Set up the data system to perform a 25 uL injection. 12 Configure the syringe. Make sure the plunger speeds on
the injector are still set properly.

13 Recheck the injector timings. See the step above.
258
Advanced User Guide
Inlets
14 Set a new vent time and initial inlet temperature time
based on the new time the needle spends in the syringe.

15 Make a 25 uL injection of your standard. Again, you
should see 5 times the response. If not, see step 13.

16 If you need more response, repeat steps 10 through 15 to
increase to larger volume. See the next section. Try performing 5 x 5 uL injections, then 5 x 50 uL injections.
Multiple injections with the PTV inlet

The preferred technique for concentrating analytes in the inlet liner is to use a single, large volume injection. Using a high capacity syringe and one septum puncture reduces the possibility of contamination and generally improves results when compared against a multiple septum puncture technique. However, if needed, you can perform multiple septum punctures during the vent time. This technique requires an Agilent data system and automatic liquid sampler.
Data system requirements

An Agilent data system is necessary for multiple injection because the needed parameters are not available through the GC keyboard.
GC ChemStation MSD ChemStation EZChrom
Software revision B.04.01 SP1 or later. Software revision E.02.00 SP2 or later
Software revision 3.3.2 or later
Setting parameters for the inlet in solvent vent mode

Set or configure the following parameters in the data system's 7890A GC method editor. Syringe size Verify the syringe size is configured correctly. The configured syringe size changes the available choices for injection volume. Injection volume Select the injection volume, then enter a number of injections. The total injection volume will be displayed. Multiple Injection Delay A pause time, in seconds, between injections. This is added to the minimum hardware cycle time.
Advanced User Guide
259
Inlets
Preinjection washes and pumps are performed only before the first injection of a multiple injection set. Postinjection washes are performed only after the last injection in a multiple injection set.
An example
These values were used for a sample with a broad range of boiling points. Table 46
Name Sample Mode MMI liner Injection volume Injection speed Column Column flow
General parameters
Value C10 to C44 hydrocarbons in hexane Solvent vent Glass wool packed One 10.0 L injection (25 L syringe) Fast 30 m x 320 m x 0.25 m -5, part number 19091J-413 4 mL/min constant flow
Table 47
Name Initial temp Initial time Rate 1 Final temp 1 Final time 1 Rate 2 Final temp 2 Final time 2
Inlet parameters
Value 40 C 0.3 min 720 C/min 450 C 5 min 100 C/min 250 C 0 min Name Rate 2 (off) Pressure Vent pressure Vent flow Vent end time Purge time Purge flow 15.6 psig 0.0 psig 100 mL/min 0.2 min 2.0 min 50 mL/min Value
Table 48
Name Initial temp Initial time
Oven parameters
Value 40 C 2.5 min
260
Advanced User Guide
Inlets
Table 48
Name Rate 1 Final temp 1 Final time 1 Rate 2 (off)
Oven parameters
Value 25 C/min 320 C 10.0 min
Table 49
Name Detector Detector temp Hydrogen flow Air flow Makeup (N2)
Detector parameters
Value FID 400 C 40 mL/min 450 mL/min 45 mL/min
Advanced User Guide
261
Inlets
C20
These results were compared with a splitless analysis of the same sample, which should produce 100% recovery of all analytes. The data showed that, under these conditions, compounds above C20 were completely recovered and that the recovery was independent of injection size. Compounds lower than C20 were partially vented with the solvent.
Possible adjustments
Depending on what you are trying to accomplish, you have a number of possible adjustments available. To eliminate more solvent Increase the vent end time, inlet initial time, and purge time. This will not affect analytes that are quantitatively trapped but will eliminate more of the solvent peak. Increase the vent flow to sweep the liner more rapidly with the same inlet timing. Increasing vent flow raises vent pressure if it is set to 0. This puts more solvent onto the column.
262
Advanced User Guide
Inlets
Raise the inlet initial temperature to vaporize more solvent and allow more to be eliminated. This also increases the loss of volatile analytes since their vapor pressures also increase. To improve recovery of low boiling analytes Reduce inlet temperature to lower the vapor pressure of the analytes and trap them more effectively. This also reduces solvent vapor pressure and more time will be needed to eliminate it. Use a retentive packing in the liner. Materials such as Tenax permit higher recovery of volatile analytes but may not release higher boiling compounds. This must be considered if quantitation on these high boiling peaks is desired. Leave more solvent in the liner. The solvent acts as a pseudo stationary phase and helps retain volatile analytes. This must be balanced against the detectors tolerance for solvent.
An examplecontinued
The single injection example shown on the last few pages makes it clear that a 10 L injection does not overload the glass wool packed liner. This means that multiple 10 L injections are possible. It was decided to make 10 injections per run, each of 10 L size. This would increase analytical sensitivity substantially. No adjustments were made to improve recovery of the low boilers since the purpose of this analysis was to detect and measure the high boiling components. After timing a trial set of 10 injections, the total time for the multiple injection set was measured to be approximately 1.3 minutes. The following timing changes were made: Table 50
Parameter Inlet Init time Vent end time Purge time Oven Init time
Modifications
Increased from 0.3 minutes 0.2 minutes 2.0 minutes 2.5 minutes To 1.6 minutes 1.5 minutes 3.0 minutes 3.0 minutes
Advanced User Guide
263
Inlets
The result is shown in the next figure. Note the difference in the vertical scale (5000 versus 500).
C20
264
Advanced User Guide
Inlets
About the Volatiles Interface

The volatiles interface provides a simple, reliable way to introduce a gas sample into your GC from an external device such as a headspace, purge and trap, or air toxic sampler. Manual syringe injections cannot be made with this interface. The interface has a small volume and is highly inert, ensuring high sensitivity and resolution for applications requiring trace level detection. The figure shows the pneumatics in the split mode.
EPC Module
Frit Valve Valve Valve PS FS
Frit
PS
Frit
Gas Sampling Valve Headspace Purge and Trap Split Vent Trap
Column
Total flow to the interface is measured by a flow sensor and is divided into two streams. One stream connects to the septum purge regulator; the other connects to a frit block. At the frit block, the flow is further divided. The first stream
Advanced User Guide
265
Inlets
goes to the gas- phase sampler and from there is introduced into the interface. The second stream, called the pressure sensing line, passes through the frit block and is measured by a pressure sensor. This stream also provides a trickle flow to the interface.
VI operating modes
There are three modes of operationsplit, splitless, and direct. The pneumatics differ for each operating mode and are discussed in detail in the rest of this document. Table 51 summarize some issues to consider when choosing an operating mode. Specifications for the interface are also listed. Table 51
Mode Split Splitless Direct
Overview of the volatiles interface

Sample concentration High Low Low Sample to column Very little, most is vented All All Can switch to split mode electronically. Must physically disconnect split vent, plug the interface, and reconfigure the GC. Maximizes sample recovery and eliminates possibility of contamination to pneumatic system. Comments
Table 52
Specification
Specifications of the volatiles interface

Value/Comment
Deactivated flow path Volume Internal dimensions Maximum flow to interface Split range 32 L 2 mm by 10 mm 100 mL/min Depends on column flow Typically no split to 100:1
266
Advanced User Guide
Inlets
Table 52
Specification
Specifications of the volatiles interface (continued)

Value/Comment 10 C above ambient (with oven at ambient) to 400 C transfer line temperature of the external sampling device
Temperature range Recommended temperature:
About the VI split mode

When you introduce a sample in the split mode, a small amount of the sample enters the column while the major portion exits from the split vent. The ratio of split flow to column flow is controlled by the user. The split mode is primarily used for high concentration samples when you can afford to lose most of the sample out the split vent and for samples that cannot be diluted.
Split ratio
Because of the interfaces small internal volume, the maximum total flow to the interface is 100 mL/min. This maximum flow puts some restriction on the split ratio you can set. Table 53 Maximum split ratios
Column flow (mL/min) 1 5 Maximum split ratio 100:1 20:1 Total flow (mL/min) 100 100
Column diameter (mm) 0.20 0.53
Split mode pneumatics

During Pre Run, during sampling, and after sampling, total flow to the interface is measured by a flow sensor and controlled by a proportional valve. Flow at the head of the column is backpressure regulated. Pressure is sensed upstream from the proportional valve.
Advanced User Guide
267
Inlets
Split
Septum Purge
EPC Module
Frit
PS
Frit
Gas Sampling Valve Headspace Purge and Trap Split Vent Trap
Column
Setpoint dependencies
Some setpoints are interdependent. If you change one setpoint, other setpoints may change to compensate. With a defined capillary column, setting column flow or linear velocity will set the inlet pressure. Table 54 Setpoint dependencies
These setpoints change Column defined Pressure Column flow* Split flow Total flow Column not defined No changes
When you change
268
Advanced User Guide
Inlets
Table 54
Setpoint dependencies (continued)

These setpoints change Column defined Column not defined not available
When you change
Column flow*
Pressure Split flow Total flow Split ratio Total flow Split flow Total flow Split flow Split ratio
Split flow Split ratio Total flow
not available not available No changes
* This setpoint appears in [Col 1] or [Col 2].
Initial values
Use the information in Table 55 to help you set up the operating conditions for your interface. Table 55
Parameter Oven initial time Interface temperature Gas saver time Gas saver flow
Suggested starting values

Allowed setpoint range 0 to 999.9 minutes Suggested starting value After sample on column
Ambient + 10 C to 400 C Transfer line temperature 0 to 999.9 minutes 15 to 100 mL/min After sample on column 15 mL/min greater than maximum column flow
Setting parameters for the split mode

Mode:
The current operating modesplit Actual and setpoint interface temperatures
Temperature
Pressure Actual and setpoint interface pressure. Controls capillary column flow.
Advanced User Guide
269
Inlets
Split ratio The ratio of split flow to column flow. Column flow is set using [Col 1] or [Col 2]. This parameter is not available if your column is not defined. Split flow Flow, in mL/min, from the split vent. This parameter is not available if your column is not defined. Total flow actual
The total flow into the interface, both setpoint and
On to reduce split vent flow at Saver time Reduced split vent flow, at least 15 mL/min. Time when flow is reduced to save gas

1 Press [Front Inlet] or [Back Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Split. 3 Set the interface temperature. 4 If you want a specific split ratio, scroll to Split ratio and
enter that number. The split ratio will be calculated and set for you.
6 If desired, turn Gas saver on. Set Saver time after the
sample has been introduced.

7 If Gas saver is on, be certain Auto prep run is On (see Pre
Run and Prep Run on page 176) or press [Prep Run] before introducing the sample.

1 Press [Front Inlet] or [Back Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Split. 3 Set the interface temperature. 4 Set Total flow into the interface. Measure flow out of the
split vent using a flow meter.

5 Subtract the split vent flow from Total flow. Subtract the
septum purge flow from the result to get column flow.
270
Advanced User Guide
Inlets
Adjust as needed.
7 If desired, turn Gas saver on. Set Saver time after the
sample has been introduced.

8 If Gas saver is on, be certain Auto prep run is On (see Pre
Run and Prep Run on page 176) or press [Prep Run] before introducing the sample.
About the VI splitless mode

This mode is used to concentrate sample at the head of the GC column during desorb. Purge timing delay must take into consideration the volume of the loop or trap in the external sampler plus the transfer line versus desorb/total flow rate. Cryo focussing is required for very volatile samples in splitless mode. When you introduce a sample, the split valve remains closed while the sample enters the interface and is transferred to the column. At a specified time after the sample is introduced, the split valve opens.
Splitless mode pneumatics

Before Pre Run When the GC is preparing for sample introduction, total flow to the interface is measured by a flow sensor and controlled by a proportional valve. Column flow is controlled via backpressure regulation. The split valve is open.
Advanced User Guide
271
Inlets
Split
Septum Purge
EPC Module
Frit Valve Valve Valve PS
Frit
FS
PS
Frit
Split Vent Trap
Gas Sampling Valve Headspace Purge and Trap
Column
During sampling Pressure upsets caused by switching valves and trap restrictions in the external sampling device can cause fluctuations in column flow rates. To compensate for this, the interface is flow controlled during sampling time. The sampling flow rate is calculated from the pressure setpoint that is active when sample introduction begins. This flow control starts when the GC goes into the Pre Run state (when your system is automated and the Pre Run light is on or during manual operation when you press [Prep Run]) and ends after the interfaces Sampling end setpoint expires.
Sampling end is required for purge and trap or thermal desorption systems and should be set the sampler desorb time.
272
Advanced User Guide
Inlets
During this user- specified sampling period, the solenoid valve is closed. Flow to the interface is measured by a flow sensor and controlled by a proportional valve.
EPC Module
Frit
PS
Frit
Split Vent Trap
Column
After sampling end The solenoid valve opens. The system returns to the Before Prep Run state. Flow to the interface is again measured by a flow sensor and controlled by a proportional valve while column flow is controlled via backpressure regulation. The purge flow is controlled by the user. If desired, gas saver can be turned on at the end of the run.
Advanced User Guide
273
Inlets
Setpoint dependencies
Some setpoints in the flow system are interdependent. If you change one setpoint, other setpoints may change to compensate. Table 56 Setpoint dependencies
These setpoints change Column defined Purging Column not defined You can change the Pressure and Total flow setpoints; other setpoints are not affected. Total flow** Total flow** Column flow* Pressure Total flow** You can change the Pressure setpoint; other setpoints are not affected.
When you change
Purge flow Pressure Column flow*
Before and after sampling, not purging
Pressure Column flow*
Column flow* Total flow** Pressure Total flow**
During sampling: You cannot change pressure and flow setpoints during sampling time.
* This setpoint appears in the column parameters. **This value is actual only.
Initial values
The table shows recommended starting values for selected parameters.
274
Advanced User Guide
Inlets
Table 57
Parameter

Allowed setpoint range 0 to 999.9 minutes Suggested starting value Interface purge time
Oven initial time Interface temperature Interface sampling end Interface purge time Gas saver time Gas saver flow
Ambient + 10 C to 400 C Transfer line temperature 0 to 999.9 minutes 0 to 999.9 minutes 0 to 999.9 minutes 15 to 100 mL/min Must be after purge time 15 mL/min greater than maximum column flow 0.2 minutes longer than introduction time
Setting parameters for the VI splitless mode

Mode:
The current operating modesplitless
Temperature Actual and setpoint interface temperatures. Column temperature must be low enough to cold trap the volatile sample. Cryo focussing is recommended. Sampling end The sample introduction interval, in minutes. The flow rate is calculated from the pressure setpoint that is active at the start of sample introduction.
Set the sampling end setpoint 0.2 minutes longer than the time the sampler needs to introduce the sample. For example, the 7694 headspace sampler has an Inject time parameter which controls how long the valve remains in the inject position. If Inject time is 1 minute, the sampling end setpoint should be set to 1.2 minutes. If youre using an 7695 Purge and Trap Concentrator, set Sampling end 0.2 minutes longer than the Desorb time parameter. If your column is defined and you specify a flow or pressure program for your column, the ramp does not begin until after the sampling end setpoint expires.
Pressure or kPa.
Actual and setpoint interface pressure in psi, bar,
Purge time The time, after the beginning of the run, when purging resumes. Purge time must be greater than Samplg end.
Advanced User Guide
275
Inlets
Purge flow The flow, in mL/min, from the split vent at Purge time. You will not be able to access or specify this value if your column is not defined. Total flow When your column is defined, Total flow displays the actual flow to the interface. You cannot enter a setpoint. If your column is not defined, Total flow will have both setpoint and actual values during purge time. All other times, the actual flow to the interface is displayed. Septum Purge 15 mL/min. Gas saver Saver flow
Flow through the septum purge vent, at least
On to reduce split vent flow at Saver time. Flow through the split vent after Saver time.
These instructions apply to both column defined and not defined.

1 Press [Front Inlet] or [Back Inlet]. 2 Scroll to Mode: and press [Mode/Type]. Select Splitless. 3 Set the interface temperature and a sampling end time. 4 If your column is defined, enter a Purge time and Purge
flow. Turn Gas saver on if desired. Set the Gas saver time after the purge time and enter a Gas saver flow.
5 If your column is not defined, enter a Purge time (Purge
flow is not available). Set Total flow greater than column flow plus septum purge flow to guarantee adequate column flow.
6 Make certain Auto Prep Run is On (see Pre Run and Prep
Run on page 176) or press [Prep Run] before introducing a sample.
About the VI direct mode

Direct sample introduction permits a quantitative transfer of analyte without risking contamination to the pneumatic system. It provides the sensitivity required for air toxic analyses. The interfaces minimal dead volume also eliminates the potential interaction of solutes with poorly swept, active surfaces. To operate in the direct mode, you must physically disconnect the split vent and reconfigure the GC.
276
Advanced User Guide
Inlets
Before Pre Run

The interface is forward pressure controlled; pressure is sensed downstream from the flow proportional valve.
EPC Module
Frit Valve Valve PS FS PS
Frit
Frit
Column
During sampling
Pressure upsets caused by switching valves in the external sampler can cause fluctuations in column flow rates. To compensate for this, the interface is flow controlled during sampling time. The sampling flow rate is calculated from the pressure setpoint that is active when sample introduction begins. This flow control starts when the GC goes into the Pre Run state (when your system is automated and the Pre Run light is on or during manual operation when you press [Prep Run]) and ends after the interfaces Sampling end setpoint expires.
Advanced User Guide
277
Inlets
Flow to the interface is measured by a flow sensor and controlled by a proportional valve.
EPC Module
Frit Valve Valve PS FS
Frit
PS
Frit
Column
After sampling end

The interface is forward pressure controlled; pressure is sensed downstream from the proportional valve. The system returns to the idle state.
278
Advanced User Guide
Inlets
Preparing the Interface for Direct Sample Introduction

Before you can operate your interface in direct mode, you must: Disconnect the split vent line Configure the GC for a direct injection
Disconnecting the split vent line

WA R N I N G Be careful! The interface may be hot enough to cause burns.
1 Press [Front Inlet] or [Back Inlet]. Turn off the interface
temperature and pressure and allow the interface to cool.

2 If desired, remove the transfer line by loosening the hex
nut with a wrench.

3 Remove the clamping plate from the interface by
loosening the captive screw with a screwdriver. Put the plate in a safe place.
4 Carefully lift the interface out of the heater block.
Advanced User Guide
279
Inlets
5 Loosen the hex nut connecting the split vent line to the
interface until you can remove the line. Put the line aside. You do not need to plug it.
6 Install a blanking nut into the split line port and
finger- tighten the nut. Tighten the nut an additional 1/4- turn using two wrenches in opposition.
7 Place the interface in the heater block. Replace the
clamping plate you removed earlier and tighten the screw until snug. Do not overtighten. If you removed the transfer line, replace it.
280
Advanced User Guide
Inlets
8 Restore the GC to normal operating conditions. Perform a
leak test on the interface fittings.
Configuring for direct mode

The GC cannot sense the presence of the split vent. When you disconnect or reconnect the vent, you must configure the GC so that the pneumatics work properly.
1 Press [Config] [Back Inlet] or [Config] [Front Inlet]. 2 Scroll to Mode and press [Mode/Type]. 3 Select Split vent removed. Press [Enter]. 4 Press [Back Inlet] or [Front Inlet]. If the inlet is correctly
configured, you will see the Direct injection display.
VI direct mode setpoint dependencies

Some setpoints in the flow system are interdependent. If you change one setpoint, other setpoints may change to compensate. Table 58 Setpoint changes
These setpoints change Column defined Before and after sampling Pressure Column flow* Total flow** Column not defined The Column flow* setpoint is not available. You can change the pressure setpoint; other setpoints are not affected.
When you change
Column flow*
Pressure Total flow**
Advanced User Guide
281
Inlets
Table 58
Setpoint changes (continued)

These setpoints change Column defined Column not defined
When you change
During sampling
You cannot change pressure and flow setpoints during sampling time.
* This setpoint appears in the column parameters .**This value is actual only
VI direct mode initial values

Use the information in Table 59 to help you set up the operating conditions for your interface. Table 59
Parameter Oven initial time Interface temperature Interface sampling end

Allowed setpoint range 0 to 999.9 minutes Ambient + 10 C to 400 C 0 to 999.9 minutes Suggested starting value interface sampling end transfer line temperature 0.2 minutes longer than actual sampling time
Setting parameters for the VI direct mode

Temperature
Actual and setpoint interface temperatures
Sampling end The sample introduction interval, in minutes. The flow rate is calculated from the pressure setpoint that is active at the start of sample introduction.
Set Sampling end 0.2 minutes longer than the time the sampler needs to introduce the sample. For example, the 7694 headspace sampler has an Inject time parameter which controls how long the valve remains in the inject position. If Inject time is 1 minute, Sampling end should be set to 1.2 minutes. If youre using a 7695 Purge and Trap Concentrator, set Sampling end 0.2 minutes longer than the Desorb time parameter. If your column is defined and you specify a flow or pressure program for your column, the ramp does not begin until after Sampling end expires.
282
Advanced User Guide
Inlets
Pressure Actual and setpoint interface pressure before a run and after sampling time. Total flow The actual flow to the interface. This is a reported value, not a setpoint. Septum Purge Flow through the septum purge vent, range 0 to 30 mL/min.
These instructions apply to both column defined and column not defined.
1 Press [Front Inlet] or [Back Inlet]. 2 Confirm that your GC is configured for direct injection. 3 Set the interface temperature. 4 Set Sampling end at 0.2 minutes longer than the sample
introduction time.
5 Make certain Auto Prep Run is On (see Pre Run and Prep
Run on page 176) or press [Prep Run] before introducing a sample.
Advanced User Guide
283
Inlets
284
Advanced User Guide
9 Columns and Oven

About the Oven 286 Oven safety 286 Configuring the Oven 287 Cryogenic Operation 288 Cryogenic setpoints 288 About Oven Temperature Programming 290 Programming setpoints 290 Oven ramp rates 291 Setting the oven parameters for constant temperature 292 Setting the oven parameters for ramped temperature 292 About the Oven Insert 294 Selecting the correct packed glass column type 295 About the column modes 295 Select a column mode 296 Setting the column parameters for constant flow or constant pressure 297 Enter a flow or pressure program (optional) 297 Programming column pressure or flow 298 About Columns 295 Backflushing a Column 299 Backflushing when connected to an MSD 299 Nickel Catalyst Tube 305 About the nickel catalyst tube 305 Gas flows 305 Setting temperatures for the nickel catalyst tube 306
285
Columns and Oven
About the Oven

Table 60
Capability Temperature range Maximum temperature Temperature programming Maximum run time Temperature ramp rates
Oven capabilities
Range 80 C (liquid N2) or 40 C (CO2) to the configured limit 450 C Up to six ramps 999.99 minutes 0 to 120 C/min, depending on instrument configuration
Oven safety
For safety, opening the oven door turns off power to the oven heater, fan, and cryogenic valve (if installed) but maintains the setpoints in memory. Closing the oven door returns the oven to normal operation. If the oven cannot attain or maintain an entered setpoint temperature during normal above- ambient operation, a problem is assumed and the oven is switched off. Possible problems include: The oven vent flaps not working The oven fan, heater, or temperature sensor not working properly An electronic problem When a shutdown occurs, the Off line in the oven parameter list blinks and the oven remains off until switched on again by pressing [Oven] [On] or by editing the Temperature setpoint.
286
Advanced User Guide
Columns and Oven
Configuring the Oven

Oven configuration sets maximum temperature, equilibration time the cool down mode, and the cryogenic setpoints, if cryo is installed.
Maximum temperature Maximum allowable oven temperature setpoint. Some accessories, such as the valve box, valves and columns have specific temperature limits. When configuring Maximum temperature, these limits should be considered so that the accessories are not damaged. Oven setpoints are verified as they are entered; a message is displayed when an entered setpoint is inconsistent with a previously defined maximum. Equilibration time The time required for the oven temperature to equilibrate after temperature is modified. Equilibration time begins when the actual oven temperature comes within 1 C of the oven temperature setting. The Equilibration time setpoint can be 0 to 999.99 minutes. Cryo
See Cryogenic Operation. Press the GC [Info] key for details.
External oven mode
Slow oven cool down mode During the oven cooling period, the fan can operate at full speed or at a reduced speed. This parameter makes the choice.
Advanced User Guide
287
Columns and Oven
Cryogenic Operation
The cryogenic valve lets you operate the oven below ambient temperature. Minimum attainable oven temperature depends on the type of valve installed. The GC senses the presence and type of cryogenic valve and disallows setpoints if no valve is installed. When cryogenic cooling is not needed or cryogenic coolant is not available, the cryogenic operation should be turned off. If this is not done, proper oven temperature control may not be possible, particularly at temperatures near ambient.
Cryogenic setpoints
Equilibration time Cryo
Set from 0 to 999.999 minutes.
[ON] enables cryogenic cooling, [OFF] disables it.
Quick cryo cool This is separate from Cryo. Quick cryo cool cools the oven faster after a run than it would without assistance. This is useful when maximum sample throughput is necessary, however it does use more coolant. Quick cryo cool turns off soon after the oven reaches its setpoint and Cryo takes over, if needed. Ambient temp The temperature in the laboratory. This setpoint determines the temperature at which cryogenic cooling is enabled.
Ambient temp + 25 C, for regular cryo operation Ambient temp + 45 C, for Quick Cryo Cool.
Cryo timeout Cryo timeout occurs, and the oven shuts off, when a run does not start within a specified time (10 to 120 minutes) after the oven equilibrates. Turning cryo timeout Off disables this feature. We recommend that it be turned On because cryo timeout conserves coolant at the end of a sequence or if automation fails. Cryo fault Shuts the oven down if it does not reach setpoint temperature after 16 minutes of continuous cryo operation. Note that this is the time to reach the setpoint, not the time to stabilize and become ready at the setpoint. For example, with a cool on- column inlet and cryo control in the track oven mode, it may take the oven 20 to 30 minutes to achieve readiness.
288
Advanced User Guide
Columns and Oven
If the temperature goes below the minimum allowed temperature (90 C for liquid nitrogen,70 C for liquid CO2), the oven will shut down.
External oven mode Isothermal internal mode and programmed external oven used to calculate column flow. Slow oven cool down mode during cool down.
On to run oven fan at slow speed
Advanced User Guide
289
Columns and Oven
About Oven Temperature Programming

You can program the oven temperature from an initial temperature to a final temperature using up to 20 ramps during a run. A single ramp temperature program raises the initial oven temperature to a specified final temperature at a specified rate and holds at the final temperature for a specified period of time.
Final temperature 1 Final time 1
Rate 1 Rate 2 = 0 Initial time 1 Initial temperature
The multiple- ramp temperature program is similar. You can program the oven from an initial temperature to a final temperature, but with various rates, times, and temperatures in between. Multiple ramps can also be programmed for temperature decreases as well as increases.
Final temperature 2 Rate 2 Final temperature 1 Rate 1 Initial time 1 Final time 1 Rate 3 = 0 Final time 2
Initial temperature
Programming setpoints
Temperature Starting temperature of a temperature programmed run. When the program begins, this value is copied into a temporary setpoint called Init temp. At the end of the run, Temperature is reset to the value in Init temp and the oven returns to its starting temperature. Initial time Time in minutes that the oven will stay at the starting temperature after a programmed run has begun. Rate The rate in C/min at which the oven will be heated or cooled.
290
Advanced User Guide
Columns and Oven
Final temperature Temperature of the oven at the end of a heating or cooling rate. Final time Time in minutes that the oven will be held at the final temperature of a temperature- programmed rate.
Total length of a run is determined by its oven temperature program. The maximum allowable time for a run is 999.99 minutes. If the program is still running at that time, the run terminates.
Post run
This function can be used with both isothermal and programmed methods. Post run is a period that begins at the end of the normal run. The parameters are: TimeHow long is the post run period? TemperatureWhat is the oven temperature during the post run period? Column pressuresWhat are the pressures at the column ends? Post run may be used to clean out a column in preparation for the next run, backflush a column to eliminate high- boilers, and other functions. When the Post run Time elapses, the GC returns to the initial state defined in the current method. If it uses cryogenic cooling and you do not start another run quickly, you could waste considerable coolant while waiting for the next run. A solution is to use a sequence that loads a less wasteful method.
Oven ramp rates

To use the fast oven ramp rates (a 240 V power option is required), your electric service must be able to supply 200 V at 15 Amp. The highest rate that you can achieve depends on many factors, including the room temperature, temperatures of the inlets and detectors, the amount of material inside the oven (columns, valves, etc.), and whether or not this is the first run of the day. The optional oven insert for fast chromatography (see About the Oven Insert on page 294), increases oven ramp rates for the back column. Table 61 lists typical oven ramp rates.
Advanced User Guide
291
Columns and Oven
Table 61
Oven ramp rates

100/120 V oven ramp rate (C/minute) 200/220/230/240 V oven ramp rate (C/minute) With optional insert 120 120 110 80 65
Temperature range (C) 50 to 70 70 to 115 115 to 175 175 to 300 300 to 450
Without insert 75 45 40 30 20
With optional Without insert insert 120 95 65 45 35 120 95 65 45 35
Setting the oven parameters for constant temperature

An isothermal run is one in which the oven is maintained at a constant temperature. For an isothermal run, set Rate 1 to zero.
1 Press [Oven] to open the oven parameter list. 2 Enter the oven temperature for the isothermal run. 3 Enter the number of minutes (Initial time) that you want
the oven to stay at this temperature. This time is the duration of the run.
4 If Rate 1 is not already 0, enter zero for an isothermal run.
Setting the oven parameters for ramped temperature

Single ramp
1 Press [Oven] to open the oven parameter list. 2 Enter a starting temperature (Temperature). 3 Enter the time (Initial time) that you want the oven to stay
at Temperature.
4 Enter the rate (Rate 1) at which the oven temperature is
to change.
5 Enter the final temperature (Final temperature 1). 6 Enter the time (Final time 1) the oven is to hold Final
temperature 1.
7 To end the oven ramp program after Ramp 1, set Rate 2 to
zero.
292
Advanced User Guide
Columns and Oven
Multiple ramps
In a multiple- ramp program, Final time for one ramp is also Initial time for the next ramp. Thus, there is only one Initial time.
1 Set up the first oven ramp as described in Single ramp. 2 Enter the rate (Rate 2) at which you want the oven
temperature to increase for the second oven ramp.

3 Enter the final temperature (Final temperature 2). 4 Enter the number of minutes (Final time 2) that you want
the oven to hold the final temperature.

5 To end the temperature program after the second ramp,
set Rate 3 to zero.

6 To add additional oven ramps, repeat the steps described.
Advanced User Guide
293
Columns and Oven
About the Oven Insert

The Oven Insert for Fast Chromatography reduces the oven volume so that the column and sample heat more quickly, yielding faster separation and faster chromatography. Furthermore, the smaller volume oven cools faster than a full- sized oven, reducing the overall analytical cycle time.
Carrying strap WARNING! Metal parts may be hot enough to burn.
The oven insert is used with any inlet, column, and detector mounted in the back position. It is not compatible with any accessory which obstructs access to the front of the oven or which requires the use of either the front inlet or the front part of the oven.
294
Advanced User Guide
Columns and Oven
About Columns
In all GCs, a samplewhich is a mixture of several componentsis vaporized in an inlet, separated in a column, and examined in a detector. The column separates components in time because: When a vaporized component is presented with a gas phase and a coating phase, it divides between the two phases according to its relative attraction to the two phases. The attraction can be solubility, volatility, polarity, specific chemical interaction, or any other property that differs from one component to another. If one phase is stationary (the coating) and the other is moving (the carrier gas), the component will travel at a speed less than that of the moving phase. How much less depends on the strength of the attraction. If different components have different attractions, they will separate in time.
Selecting the correct packed glass column type

This topic is covered in the Maintenance manual. See To attach a packed column to the purged packed inlet for details.
About the column modes

The flow modes available are determined by the GC inlets control mode. When the inlets control mode is set to Pressure control, all of the flow modes and pressure modes below are available for the column. When the inlets control mode is set to Flow control, the columns mode is not selectable. For an inlets mode of Flow control, only column flow can be entered.
The flow modes

Flow rates are corrected to NTP (normal temperature and pressure, 25 C and 1 atmosphere.
Advanced User Guide
295
Columns and Oven
Constant flowMaintains a constant mass flow rate of carrier gas in the column throughout the run. If the column resistance changes due to a temperature program, the column head pressure is adjusted to keep the flow rate constant. This can shorten runs significantly. Ramped flowIncreases the mass flow rate in the column during the run according to a program you enter. A column flow profile can have up to three ramps, each consisting of a programmed increase followed by a hold period.
The pressure modes

The pressure modes are not available if the column is not defined or the inlets mode is set to Flow control. Pressures are gauge pressuresthe difference between the absolute pressure and the local atmospheric pressure. Because most detectors present little resistance to the column flow, the gauge pressure at the column head is usually the same as the pressure difference between column inlet and exit. The mass selective detector and the atomic emission detector are the exceptions. Constant pressureMaintains a constant gauge pressure at the head of the column throughout the run. If the column resistance and gas density changes during a run, the gauge pressure does not change but the mass flow rate does. Ramped pressureIncreases the column head gauge pressure during the run according to a program you enter. A column pressure profile can have up to three ramps, each consisting of a programmed increase followed by a hold period.
Select a column mode

The columns mode parameter is not available if the inlets mode parameter is set to Flow control. When a splitter controlled by a PCM or AUX pressure is used to divide flow between multiple columns, only the mode setting of the lowest column number configured determines the mode used. All other column mode settings exiting the splitter are ignored by the GC.
1 Press [Col 1] or [Col 2], or press [Aux col #] and enter the
column number.
2 Scroll to the Mode line.
296
Advanced User Guide
Columns and Oven
3 Press [Mode/Type] to see the column mode list. 4 Scroll to the column mode you want. Press [Enter].
This completes column mode selection. Next you must specify the inlet conditions either during the entire run (if you selected either of the constant modes) or at the beginning of the run (if you selected either of the ramped modes).
Setting the column parameters for constant flow or constant pressure

If the column is defined, you can enter any one of these quantitiesthe GC will calculate and display the other two. For example, you may have selected Constant pressure as the column mode. You decide to specify, as a starting condition, the column flow. The GC will compute the pressure necessary to achieve this flow (as well as the average linear velocity) and hold this pressure constant during the run. If you select Constant flow as the mode and specify column flow as the initial condition, the GC will still calculate the pressure necessary to achieve this flow, but it will adjust the pressure as necessary to maintain constant flow. If the column is not defined, you can enter only pressure. Constant flow can still be specified, but the GC cannot know what the flow is.
column number.
2 Scroll to the Pressure or Flow or Velocity line. 3 Type the desired initial value, followed by [Enter]. The GC
will compute and display the other two values. Adjust them, if you choose to, by repeating steps 2 and 3 but note that changing any one changes all three. This completes setting the initial carrier gas condition.
Enter a flow or pressure program (optional)

If you selected either the ramped pressure or ramped flow column mode, the column parameter list contains entries for setting up a ramp program. You begin with an initial value, either Initial Pressure or Initial Flow, and an Initial time. At the end of that time, Rate 1 begins and runs until it reaches Final pressure (or Final flow). It
Advanced User Guide
297
Columns and Oven
remains at that value for Final time 1. You can then add a second and third ramp, each consisting of a Rate, a Final value (pressure or flow), and a Final time. The program ends when it reaches a Rate that is set to 0 (Off). When a flow or pressure program is running, the Pressure, Flow, and Velocity lines that you used to set constant conditions show the progress of the program. The oven program determines the length of the run. If a flow or pressure program ends before the analytical run does, the flow (or pressure) remains at the last final value.
Programming column pressure or flow

column number.
2 Scroll to Initial pressure (or Initial flow). Type the desired
value and press [Enter].

3 Similarly, enter a value for Initial time. This completes the
initial part of the program.

4 To begin a ramp, enter a positive value for Rate 1. It does
not matter whether you are programming up or downthe rate is always positive.
5 If Rate 1 is zero, the program ends here. If you enter any
other value, the Final value lines for the first ramp appear and the cursor moves to the line.
6 Enter values for Final pressure 1 (or Final flow 1) and Final
time 1. This completes the first ramp.

7 To enter a second ramp, scroll to the appropriate Rate
line and repeat steps 5 and 6. A maximum of 20 ramps can be entered.
298
Advanced User Guide
Columns and Oven
Backflushing a Column
Backflush is a means of discarding high- boilers from a column after the peaks of interest have eluted. It saves analysis time and has these additional benefits: Longer column life less high temperature exposure removal of high- boilers protection from air and water at high temperatures Less chemical background ghost peaks wrap- around of late eluters from previous runs stationary phase decomposition peaks Less contamination of the mass selective detector (MSD) source, if using MSD longer time between source cleanings higher stability of calibrations You will need to experimentally determine the correct flow/pressure settings and the backflush time appropriate for your analysis. Determine the correct values by testing the backflush method, then running a blank to check for residual late eluters.
CAUTION
Only backflush an inlet that has a split vent line with a chemical trap, such as the split/splitless, PTV, and VI. Attempts to backflush using other inlet types will most likely damage the pneumatics flow modules.
Refer to the Agilent web site at http://www.agilent.com/chem for example backflush applications, especially if using an MSD.
Backflushing when connected to an MSD

If using an MSD with the GC, backflushing becomes more complex. Set up backflush as a post run event by using the Backflush Wizard present in the MSD Productivity ChemStation.
Advanced User Guide
299
Columns and Oven
Backflushing using a capillary flow technology device

Because the following capillary flow technology (CFT) devices connect to a controlled carrier gas supply, they can be used to backflush a column: G2855B Capillary Flow Technology Deans Switching System G3180B Capillary Flow Technology Two- Way Splitter (with makeup gas) G3183B Capillary Flow Technology Three- Way Splitter G3185B QuickSwap Accessory A conceptual diagram for a simple setup is shown in the figure.
Split Vent Trap
Auxiliary EPC/PCM
Detector
Inlet
CFT Device
Column
After the last analyte of interest elutes, you can program a decrease in inlet column flow with an increase in the pressure/flow from the Aux EPC or PCM connected to the CFT device, thereby reversing column flow and forcing the remaining analytes off the column and out of the inlet split vent. You can do this using a post run program or as a ramped pressure or flow program.
To set up a post run backflush

A main advantage of the postrun backflush method is that the GC turns off detection during this time. If using an MSD, this helps prevent damage to the detector and is the recommended backflush method.
300
Advanced User Guide
Columns and Oven
If using an Agilent data system, a Backflush Wizard provides a straightforward interface for making these settings.
1 Verify that all columns are properly configured. 2 Since the backflush will run as a postrun program, set
the method so that the oven program ends after the last peak of interest returns to baseline, or after reaching the last temperature of interest.
3 Press [Post Run] and enter the backflush duration as the
Time. The oven temperature and column pressure/flow setpoints for installed columns appear. Whether you can enter a pressure or flow for a column depends on its mode (pressure or flow).
4 Enter the oven temperature for the backflush. 5 Enter the backflush flow(s) or pressure(s).
If in flow mode: Enter a negative flow for the column connected between the inlet and the CFT device. The GC will automatically establish the corresponding pressures needed in the inlet and the CFT device. Increase the flow rates in the column(s) connected between the CFT device and the detector(s). If in pressure mode: Set the pressure of the column connected between the inlet and the CFT device to 0.000. This turns off flow from the inlet. Increase the pressure of the primary column connected between the CFT device and the detector(s). This creates the backward flow through the column and increases the flow through any connected detectors. When developing the backflush portion of your method, consider the following: Ensure that the split vent flow setpoint is at least 25 mL/min and at least 50% more than the column backflush flow rate. If using gas saver, ensure that the gas saver flow setpoint is at least 25 mL/min and at least 50% more than the column backflush flow rate.
Advanced User Guide
301
Columns and Oven
To backflush using a ramped pressure program

In this case, the backflush occurs as part of the run, so the detectors continue to collect data. During the backflush, you may wish to turn off data collection in the data system.
CAUTION
To avoid damage to an MSD, Agilent strongly recommends setting up backflush as a post run event, not as part of a ramped column program. If you still choose to backflush as part of a run, be very careful that the flow into the MSD does not exceed the limits of the vacuum pump.
1 Verify that all columns are properly configured. 2 Enter all method parameters for the analysis: sampler
parameters, inlet parameters, oven temperature profile, detector flows and temperatures, and so forth.
3 Program the oven for the backflush.
Include any temperature profile needed for backflush. Set the total run time to include sufficient time for backflush.
4 Program the pressure ramp for the column installed
between the inlet and the CFT device. After the last analyte elutes or after reaching the last temperature of interest, program a fast ramp (for example, 30 psi/min) with a final pressure of 0.
5 Program the pressure ramp for the primary column
installed between the CFT device and the detector. The pressure should increase slightly during the backflush duration so that the flow into the detectors remains relatively stable. If you turned off data acquisition in a data system during backflush, remember to turn it on again at the end of the run.
To backflush using a ramped flow program

In this case, the backflush occurs as part of the run, so the detectors continue to collect data. During the backflush, you may wish to turn off data collection in the data system.
302
Advanced User Guide
Columns and Oven
CAUTION
To avoid damage to an MSD, Agilent strongly recommends setting up backflush as a post run event, not as part of a ramped column program. If you still choose to backflush as part of a run, be very careful that the flow into the MSD does not exceed the limits of the vacuum pump.
1 Verify that all columns are properly configured. 2 Enter all method parameters for the analysis: sampler
parameters, inlet parameters, oven temperature profile, detector flows and temperatures, and so forth.
3 Program the oven for the backflush.
Include any temperature profile needed for backflush. Set the total run time to include sufficient time for backflush.
4 Program the flow ramp for the column installed between
the inlet and the CFT device. After the last analyte elutes or after reaching the last temperature of interest, program a fast ramp with a final flow that is negative.
5 Program the flow ramp for the primary column installed
between the CFT device and the detector. Typically hold at the methods final value for the backflush duration. If you turned off data acquisition in a data system during backflush, remember to turn it on again at the end of the run.
Backflushing using a switching valve

Backflushing is done using a column switching valve controlled by the Run Table. See Run Time Programming on page 16. The valve is plumbed as follows: Position 1 Carrier gas flows through the column to the detector. This is the normal flow path. Position 2 Carrier gas flows through the column toward the inlet, removing components on the column through the inlet vent line. The Run Table contains commands to perform these actions: After the last peak of interest appears, switch the valve to Position 2. Higher boiling peaks are discarded through the inlet vent.
Advanced User Guide
303
Columns and Oven
At the same time, turn data acquisition off. At the end of the backflush period (determined experimentally), switch the valve to Position 1 and turn data acquisition on. The system is now ready for the next run.
304
Advanced User Guide
Columns and Oven
Nickel Catalyst Tube

About the nickel catalyst tube
The Nickel Catalyst Tube accessory, G2747A, is used for trace analysis of CO and CO2 with a flame ionization detector. The gas sample is separated on the column and passed over a heated catalyst in the presence of hydrogen, which converts the CO and CO2 peaks to CH4.
Sample
Hydrogen
Air
Carrier gas
Gas sample valve
Column
Nickel catalyst
FID
Gas flows
For a standard FID installation: Table 62
Gas Carrier (helium) FID hydrogen FID air
Gas flows for a standard FID

Flow rate, mL/min 30 30 (see Caution) 400
Advanced User Guide
305
Columns and Oven
Table 63
Gas
Gas flows for a TCD/FID series installation

Flow rate, mL/min 30 25 45 (see Caution) 500
Carrier (helium) TCD switching flow FID hydrogen FID air
CAUTION
Hydrogen flow is pressure-controlled, where an FID provides a known resistance. The nickel catalyst tube increases flow resistance, so that the calibration is no longer valid. You must measure hydrogen flow with a bubble or similar meter. The nickel catalyst can be damaged by exposure to air.
Setting temperatures for the nickel catalyst tube

The nickel catalyst tube is usually mounted in the back inlet position and controlled by the back inlet temperature setpoint. For most analyses, set these temperatures: Nickel catalyst tube375 C FID400 C
306
Advanced User Guide
10 Detectors
About Makeup Gas 308 About the FID 309 About the TCD 314 About the uECD 322 About the NPD 329 About the FPD 342
307
10 Detectors
About Makeup Gas

Most detectors use a makeup gas to increase the flow rate through the detector body. This sweeps peaks out of the detector quickly, avoiding mixing of components and loss of resolution. This is particularly important with capillary columns because the column flow rates are so small. The makeup gas line of your detector parameter list changes depending on your instrument configuration. If you have an inlet with the column not defined, the makeup flow is constant. If you are operating with column defined, you have a choice of two makeup gas modes.
Constant makeup This mode provides a constant flow of makeup gas to the detector. Column + makeup = constant This mode provides a variable flow of makeup gas to the detector. As column flow increases or decreases, the makeup flow changes to provide a constant combined flow to the detector. If you choose this option, enter a value under Combined flow. The Combined flow line always displays the same value, while the Makeup line changes as the actual makeup flow changes.
To change the makeup gas flow mode

1 Press [Front Det] or [Back Det]. 2 Scroll to Mode. Press [Mode/Type]. 3 Scroll to the correct mode and press [Enter].
308
Advanced User Guide
Detectors
10
About the FID

The FID passes sample and carrier gas from the column through a hydrogen- air flame. The hydrogen- air flame alone creates few ions, but burning an organic compound increases the number of ions produced. A polarizing voltage attracts these ions to a collector located near the flame. The current produced is proportional to the amount of sample being burned. This current is sensed by an electrometer, converted to digital form, and sent to an output device. The FID uses three supply gases (hydrogen, makeup gas, and air) and two supply lines. Air flows through one supply line, while hydrogen mixed with the makeup gas flows through the other. All three supply gases use: A filter frit to protect the flow path and limit the flow rate A proportional valve to control the pressure A pressure sensor and restrictor to control the valve The hydrogen and makeup mix outside the flow module and enter the detector at the base of the jet. Air enters above the jet.
Advanced User Guide
309
10 Detectors
H2
Makeup
Air
EPC Module Frit Valve Frit Valve Frit Valve PS Vent
PS
PS
Restrictor
Restrictor
Restrictor
Column
Table 64
Property
Properties of the FID

Value/Comment 1 x 107 10 to 100 picograms of an organic compound dependent on the molecular structure. Responds to all organic compounds (C-H bonds) except those which do not burn or ionize in the hydrogen-air flame. There is little or no response for H2O, CO2, CO, N2, O2 CS2 or inert gases. Formaldehyde and heavily halogenated compounds give minimal response.
Dynamic range Sensitivity Selectivity
How FID units are displayed in Agilent data systems and on the GC
The GC displays the FID signal in picoamperes (pA). The following table lists how different data systems convert the display units to reporting units.
310
Advanced User Guide
Detectors
10
Table 65
Data system
Unit conversions
Height units 1 pA 1 x 10 pA 3.2 x 10-3 pA 1.25 x 10-4 pA
-4
LSV (height units) 1.3 x10-4 pA 1.3 x 10 pA 4.2 x 10-3 pA device dependent
-4
Area units 1 pA-sec 1 x 10 pA 3.2 x 10-3 pA 1.25 x 10-4 pA

-4
Noise (ASTM)* 0.038 pA 0.038 pA 0.038 pA 0.038 pA
Agilent data system SIGRange 0 SIGRange 5 Analog 1V
* Noise is recommended maximum when determining MDL. SIGRange used with 3393 and 3396 integrators. Analog 1V is an approximate value.
To light the FID flame

Press [Front Det] or [Back Det], scroll to Flame, then press [On/Yes].
To extinguish the FID flame

Press [Front Det] or [Back Det], scroll to Flame, then press [Off/No].
FID automatic reignition (Lit offset)

Lit offset is the expected minimum difference between the FID output with the flame lit and the output with the flame off. The GC checks this value during runs and when loading a method. During a run, if the output falls below the Lit offset value, the FID will attempt to reignite three times. If after the third attempt the output does not increase by at least this value, the detector shuts down all functions except temperature and makeup gas flow. When loading a method that includes a Flame On setting, the GC performs a similar check. If the detector output is less than the Lit offset, it will attempt reignition after reaching method setpoints. The default setting for Lit offset is 2.0 picoamps. This is a good working value for all but very clean gases and systems. You may want to lower this setpoint if the detector attempts to reignite when the flame is still on, thus producing a shutdown.
Advanced User Guide
311
10 Detectors
To change Lit offset:

1 Press [Config][Front Det] or [Config][Back Det]. 2 Scroll to Lit offset. 3 Enter the new value and press [Enter].
Recommended starting conditions for new FID methods

See Table 66 for guidelines and rules to select initial detector settings for new methods. Table 66 Recommended starting conditions
Combustible gas mix Detector temperature
Make sure that the final hydrogen-to-air ratio is between 8% and 12% Set to 20 C above the highest oven temperature, depending on the column type. A temperature of 300 C provides a good starting point and easier ignition, and minimizes water condensation. The GC will not attempt to ignite the flame at a temperature <150 C.
Carrier gas flow (hydrogen, helium, nitrogen) Packed columns Capillary columns Detector gases Standard installation Column plus capillary makeup Hydrogen Air With Nickel Catalyst Accessory: Standard installation Column plus capillary makeup Hydrogen Air With Nickel Catalyst Accessory: TCD to FID series installation Column plus capillary makeup TCD switching flow Hydrogen 24 to 60 10 to 60 30 25 45* 10 to 60 24 to 60 200 to 600 30 30* 400 10 to 60 24 to 60 200 to 600 30 30 400 Suggest 10 to 60 mL/min Suggest 1 to 5 mL/min Flow range mL/min Suggested flow mL/min
312
Advanced User Guide
Detectors
10
Table 66
Recommended starting conditions (continued)
Air
200 to 600
450
* Detector hydrogen is pressure controlled, where the detector provides a known resistance. If using a nickel catalyst tube, the resistance changes, and the flow rates displayed by the GC will not be accurate. Measure the actual hydrogen flow using a flow meter at the detector vent, with all other flows turned off.
Use nitrogen makeup gas (instead of helium) for greater sensitivity.
Setting parameters for FID

WA R N I N G Verify that a column is installed or the FID column fitting is plugged before turning on the air or hydrogen. An explosion may occur if air and hydrogen are allowed to leak into the oven.
To set the FID parameters:

1 Verify:
Makeup gas is configured Installed jet type is correct for column type
2 Press [Front Det] or [Back Det]. 3 Set the detector temperature. The temperature must be
greater than 150 C for the flame to light.

4 Set the hydrogen flow rate, if desired, and press [Off/No]. 5 Change the air flow rate, if desired, and press [Off/No]. 6 If using a packed column, set the FID makeup gas to
0.0/Off.
7 If using a defined capillary column, set the makeup gas
flow or combined column plus makeup gas flow.

8 Scroll to Flame and press [On/Yes]. This turns on the air
and hydrogen and initiates the ignition sequence. The signal typically increases to 5 to 20 pA after ignition. Verify that the flame is lit by holding a cold, shiny surface, such as a mirror or chrome- plated wrench, over the collector exit. Steady condensation indicates that the flame is lit.
Advanced User Guide
313
10 Detectors
About the TCD

The TCD compares the thermal conductivities of two gas flowspure carrier gas (the reference gas) and carrier gas plus sample components (the column effluent). This detector contains a filament that is heated electrically so that it is hotter than the detector body. The filament temperature is held constant while alternate streams of reference gas and column effluent pass over it. When a sample component appears in the effluent, the power required to keep the filament temperature constant changes. The two gas streams are switched over the filament five times per second (hence the ticking sound) and the power differences are measured and recorded. When helium (or hydrogen) is used as carrier gas, the sample causes the thermal conductivity to fall. If nitrogen is used, the thermal conductivity usually goes up because most things are more conductive than nitrogen. Because the TCD does not destroy the sample during the detection process, this detector can be connected in series to a flame ionization detector or other detector.
314
Advanced User Guide
Detectors
10
Column effluent is forced away from the filament. TCD measures reference gas.
Column effluent is forced toward the filament. TCD measures peaks (if present).
Advanced User Guide
315
10 Detectors
TCD pneumatics
This is the pneumatics design of the TCD.
Makeup Reference Gas Vent
Valve PS
EPC Module Restrictor
Frit
Frit
Valve PS Restrictor
Reference switching valve
Column
TCD carrier, reference, and makeup gas

Reference and makeup gas must be the same as the carrier gas, and the gas type must be specified in both the inlet and detector parameter lists. When using packed columns, we recommend a small makeup gas flow (2 to 3 mL/min) to get the best peak shapes. Use the next figure to select a value for reference gas flow for either capillary or packed columns. Any ratio within 0.25 of that in the figure is suitable.
316
Advanced User Guide
Detectors
10
4.0
3.0 Ratio of reference flow to column + makeup flow
2.0
1.0
0 10 20 30 40 50 60
Column + makeup flow, mL/min
TCD gas pressures

Choose a flow, find a pressure, set source pressure 10 psi (70 kPa) higher.
4
Hydrogen 3 Reference gas flow, mL/min 2
Helium
Nitrogen
Pressure (psig) (kPa)
10 69
20 138
30 207
40 276
50 345
60 414
Advanced User Guide
317
10 Detectors
20 16 Hydrogen 12 Makeup gas flow, mL/min 8 4 Helium Nitrogen
10 69
20 138
30 207
40 276
50 345
60 414
Selecting reference and makeup flows for the TCD

Table 67
Gas type Carrier gas (hydrogen, helium, nitrogen) Reference (same gas type as carrier) Capillary makeup (same gas type as carrier) Detector temperature <150 C, cannot turn on filament Detector temperature should be 30 C to 50 C greater than highest oven ramp temperature.
Recommended flow rates and temperatures

Flow range Packed, 10 to 60 mL/min Capillary, 1 to 5 mL/min 15 to 60 mL/min See the figures to select a value. 5 to 15 mL/mincapillary columns 2 to 3 mL/minpacked columns
Sample components with higher thermal conductivities than the carrier gas produce negative peaks. For example, helium or hydrogen form a negative peak with nitrogen or argon- methane as the carrier gas.
Chemically active compounds reduce TCD filament life

The tungsten- rhenium TCD filament has been chemically passivated to protect against oxygen damage. However, chemically active compounds such as acids and halogenated
318
Advanced User Guide
Detectors
10
compounds may attack the filament. The immediate symptom is a permanent change in detector sensitivity due to a change in filament resistance. If possible, such compounds should be avoided. If this is not possible, the filament may have to be replaced frequently.
Changing the TCD polarity during a run

Negative polarity On inverts the peak so the integrator or ChemStation can measure it. Negative polarity can be a run table entry; see Run Time Programming on page 16.
Detecting hydrogen with the TCD using helium carrier gas

Hydrogen is the only element with thermal conductivity greater than helium, and mixtures of small amounts of hydrogen (<20%) in helium at moderate temperatures exhibit thermal conductivities less than either component alone. If you are analyzing for hydrogen with helium carrier gas, a hydrogen peak may appear as positive, negative, or as a split peak. There are two solutions to this problem: Use nitrogen or argon- methane as carrier gas. This eliminates problems inherent with using helium as carrier, but causes reduced sensitivity to components other than hydrogen. Operate the detector at higher temperaturesfrom 200 C to 300 C. You can find the correct detector operating temperature by analyzing a known range of hydrogen concentrations, increasing the operating temperature until the hydrogen peak exhibits normal shape and is always in the same direction (negative relative to normal response to air or propane) regardless of concentration. This temperature also ensures high sensitivity and linear dynamic range. Because hydrogen peaks are negative, you must turn negative polarity on at appropriate times so the peak appears positive.
Advanced User Guide
319
10 Detectors
Setting parameters for the TCD

1 Press [Front Det] or [Back Det]. 2 Set the detector temperature. Do not set higher than the
maximum temperature allowed for the column because part of the column passes through the heated block and into the cell.
3 Verify that makeup gas type is the same as that plumbed
to your instrument (next to Makeup line in the parameter list). Change the gas type, if necessary.
4 Set the reference gas flow rate. 5 If you are using packed columns, turn off the makeup gas
(or proceed to step 6 and enter 2 to 3 mL/min, see TCD carrier, reference, and makeup gas on page 316) and proceed to step 7
6 If you are using capillary columns:, choose a flow mode and
set the makeup gas flow or combined flow.

7 Turn on the filament. Allow about 30 minutes for thermal
stabilization. A longer period may be needed for the highest sensitivity.

8 If necessary, turn Negative polarity [On/Yes] to invert
negative- going peaks. When a sample contains components giving both positive- and negative- going peaks, Negative polarity can be switched on and off during a run as a timetable event.
Example: Packed mode (packed and large capillary columns)

Column flow is 15 to 60 mL/min. Set the reference flow to 1.5 times the sum of column flow + makeup flow. Makeup gas is recommended with all capillary columns. It allows the column to be inserted all the way into the detector and withdrawn 1 mm. If makeup is not used, the column must be no more than 3 mm above the ferrule. Minimum makeup flow is 1 mL/min.
1/8-inch stainless steel column If column flow is 30 mL/min, set the reference flow to 30 1.5 = 45 mL/min. Total detector flow is 30 + 45 = 75 mL/min. 10 m 0.53 mm column If column flow is 15 mL/min and makeup flow = 2 mL/min, set the reference flow to 1.5 (15 + 2) = 25.5 mL/min. Total detector flow is 17 + 25.5 = 42.5 mL/min.
320
Advanced User Guide
Detectors
10
Example: Capillary mode (small capillary columns)

If combined column plus makeup flow is between 5 and 10 mL/min, set the reference flow at 3 the combined flow. For a combined flow between 10 and 15 mL/min, use a multiplier of 2. This will bring the TCD within 25% of the maximum response. For further optimization, adjust the reference flow.
2 m 0.2 mm capillary column If column flow is 0.75 mL/min, the makeup must be at least 4.25 mL/min. Set it = 5. Reference flow will then be 3 5.75 = 17.25 mL/min. Total detector flow = 5.75 + 17.25 = 22.5 mL/min. 25 m 0.32 mm capillary column If column flow = 10 mL/min, set makeup low to minimize sample dilution. Set it = 2 mL/min. Reference flow will then be 12 2 = 24 mL/min. Total detector flow = 12 + 24 = 36 mL/min.
Advanced User Guide
321
10 Detectors
About the uECD

The micro- cell detector (uECD) contains a cell plated with 63Ni, a radioactive isotope. The 63Ni releases particles that collide with carrier gas molecules to produce low- energy electronseach particle produces approximately 100 electrons. The free electrons produce a small currentcalled the reference or standing currentthat is collected and measured in a pulsed circuit. When a sample component molecule comes into contact with the free electrons, the electrons may be captured by the sample molecules to create negatively charged ions. The voltage across the cell electrodes is pulsed to collect the remaining free electrons while the heavier ions are relatively unaffected and swept out the vent with the carrier gas flow. Cell current is measured and compared to a reference current. The pulse rate is adjusted to maintain a constant cell current. The more uncaptured electrons, the lower the pulse frequency required to match the reference current. When a component that captures electrons passes through the cell, the pulse rate rises. This pulse rate is converted to a voltage and recorded.
uECD safety and regulatory information

The 63Ni isotope
The radioactive isotope used in the cell is 63Ni. It is plated onto the inner surface of the cell body and is solid at temperatures used in chromatography. Some other properties are listed below. Table 68
Property Halflife: Emission: Melting point: Dimensions of the active part of the uECD: Total activity (uECD cell):
Properties of 63Ni
Value 101.1 years 65.87 keV max., beta radiation 1453 C Inside diameter: 6 mm Height: 4.2 mm 555 MBq (15 millicuries) maximum
322
Advanced User Guide
Detectors
10
ECD licenses
Customers in the United states can purchase a uECD under either a General License or a Specific License. Customers outside the United States should contact their local Agilent sales office for information.
Specific License Specific License uECDs require you to obtain a Materials License from the Nuclear Regulatory Commission (NRC) or the local state agency, permitting you to possess the amount and kind of radioisotope used in the detector. You can typically ship, sell, or transfer the ECD to other Specific Licensees. If the license permits, you may also open the uECD for cleaning. General License General License uECDs do not require a Materials License. You become a General Licensee automatically when you purchase a uECD directly from Agilent Technologies. Some states may require that you register the uECD with a state agency.
Certain restrictions apply to General Licenses:
1 Owners may not open the uECD cell. 2 Owners shall not modify the cell in any manner. 3 Owners shall not use any solvent, including water, to
internally clean the cell.

4 Owners shall not interfere with or attempt to defeat the
overheat circuitry that may be supplied with the uECD.

5 Owners shall not transfer the uECD to another person or
another location except as described in the applicable Regulations.

6 Owners must perform a radioactive leak test at least
every 6 months.
7 Owners must maintain records as required by your local
Agency (the NRC or, in certain states, a state agency).

8 Owners must notify the Agency in case of incidents or
failures that might lead to a hazardous condition. Additional information is available in the publication Information for General Licensees, part no. 5961- 5664.
uECD warnings
Although beta particles at this energy level have little penetrating power the surface layer of the skin or a few sheets of paper will stop most of themthey may be
Advanced User Guide 323
10 Detectors
hazardous if the isotope is ingested or inhaled. For this reason the cell must be handled with care: Radioactive leak tests must be performed at the required intervals, the inlet and outlet fittings must be capped when the detector is not in use, corrosive chemicals must not be introduced into the detector, and the effluent from the detector must be vented outside the laboratory environment.
WA R N I N G
Materials that may react with the 63Ni source, either to form volatile products or to cause physical degradation of the plated film, must be avoided. These materials include oxidizing compounds, acids, wet halogens, wet nitric acid, ammonium hydroxide, hydrogen sulfide, PCBs, and carbon monoxide. This list is not exhaustive but indicates the kinds of compounds that may cause damage to 63Ni detectors.
WA R N I N G
In the extremely unlikely event that both the oven and the detector heated zone should go into thermal runaway (maximum, uncontrolled heating in excess of 400 C) at the same time, and that the detector remains exposed to this condition for more than 12 hours, take the following steps:
After turning off the main power and allowing the instrument to cool, cap the detector inlet and exhaust vent openings. Wear disposable plastic gloves and observe normal laboratory safety precautions. Return the cell for exchange, following directions included with the License Verification Form (part no. 19233- 90750). Include a letter stating the condition of abuse. It is unlikely, even in this very unusual situation, that radioactive material will escape the cell. However, permanent damage to the 63Ni plating within the cell is possible, and therefore, the cell must be returned for exchange.
WA R N I N G
Do not use solvents to clean the uECD.
324
Advanced User Guide
Detectors
10
WA R N I N G
You may not open the uECD cell unless authorized to do so by your local nuclear regulatory agency. Do not disturb the four socket-head bolts. These hold the cell halves together. Removing or disturbing them is a violation of the terms of the General License and could create a safety hazard.
Safety precautions when handling uECDs

Never eat, drink, or smoke when handling uECDs. Always wear safety glasses when working with or near open uECDs. Wear protective clothing such as laboratory jackets, safety glasses, and gloves, and follow good laboratory practices. Wash hands thoroughly with a mild non- abrasive cleaner after handling uECDs. Cap the inlet and outlet fittings when the uECD is not in use. Connect the uECD exhaust vent to a fume hood or vent it to the outside. See the latest revision of title 10, Code of Federal Regulations, part 20, (including appendix B) or the applicable State regulation. For other countries, consult with the appropriate agency for equivalent requirements. Agilent Technologies recommends a vent line inside diameter of 6 mm (1/4 inch) or greater. With a line of this diameter, the length is not critical.
Advanced User Guide
325
10 Detectors
uECD gas flows

Anode purge and makeup gas
Frit
Restrictor
PS
63Ni
Vent
Valve Restrictor Capillary adapter EPC Module
Column
uECD linearity
The uECD response factor versus concentration curve is linear for four orders of magnitude or more (linear dynamic range = 104 or higher) for a broad range of compounds. You should still run a calibration curve on your samples to find the limits of the linear range for your materials.
uECD detector gas

The uECD operates with either nitrogen or argon/methane as the makeup and anode gas. Purity is critical; gases must exceed 99.9995% purity. Because of the high detector sensitivity, carrier and makeup gas must be dry and oxygen- free. Moisture, chemical, and oxygen traps in good condition should be installed in carrier and makeup gas supply lines. Do not use plastic (including Teflon) tubing, plastic- bodied traps, or O- ring seals.
uECD temperature
To prevent peak tailing and to keep the cell clean, the detector temperature should be set higher than the highest oven temperature usedthe setpoint should be based on the
326
Advanced User Guide
Detectors
10
elution temperature of the last compound. If you operate at excessively high temperatures, your results will not necessarily improve and you may increase sample and column decomposition.
uECD analog output

If you intend to use the analog output from the uECD, you must set the output Range to 10.
1 Press [Analog Out 1] or [Analog Out 2]. 2 Scroll to Range. 3 Type 10 and press [Enter].
Recommended starting conditions for new uECD methods

Use the following information when selecting temperatures and flows. Maximum source pressure must not exceed 100 psi. Use the maximum source pressure to achieve maximum makeup flow rate. Table 69 Starting values
Gas Carrier gas Packed columns (nitrogen or argon-methane) Capillary columns (hydrogen, nitrogen, or argon-methane) Capillary makeup (nitrogen or argon-methane) Temperature 250 C to 400 C Detector temperature is typically set 25 C greater than the highest oven ramp temperature. Recommended flow range 30 to 60 mL/min 0.1 to 20 mL/min, depending on diameter 10 to 150 mL/min (30 to 60 mL/min typical)
uECD makeup gas notes

If the carrier gas type is different from the makeup gas type, the makeup gas flow rate must be at least three times the carrier gas flow rate. uECD sensitivity can be increased by reducing the makeup gas flow rate.
Advanced User Guide
327
10 Detectors
uECD chromatographic speed (for fast peaks) can be increased by increasing the makeup gas flow rate.
uECD temperature programming

The uECD is flow sensitive. If you are using temperature programming, in which the column flow resistance changes with temperature, set up the instrument as follows: Set the carrier gas in the Constant flow mode. Set detector makeup gas to Constant makeup. If you choose to work in the constant pressure mode, the makeup gas should be set in the Column +makeup=constant mode.
Setting parameters for the uECD

Verify that your detector gases are connected, a column is properly installed, and the system is free of leaks. Set the oven temperature and the inlet temperature and flow. Make sure your carrier gas type is the same as that plumbed to your GC.
1 Press [Front Det] or [Back Det]. 2 Set the detector temperature. To keep the uECD cell
clean, this temperature must be higher than the oven temperature.

3 Verify that the makeup gas type is the same as that
plumbed to your instrument. The gas type is in parentheses next to the Makeup line on the parameter list. Change the gas type, if necessary.
4 Enter a value for the makeup gas flow.
If you are using packed columns, turn off the makeup gas. If your capillary column is defined, choose a flow mode and set the makeup or combined gas flow. If your capillary column is not defined, only constant makeup flow is available. Enter a makeup gas flow.
328
Advanced User Guide
Detectors
10
About the NPD

New NPD features and changes
The NPD firmware in this GC (A.01.08 or higher) is considerably different from that in earlier versions and from the 6890 firmware. Major changes are: Equilibration time parameter has been removed. Adjust Offset feature has been changed. Auto Adjust on/off has been added. Dry Mode has been added. Blos/ceramic bead selector has been added. We strongly recommend that you allow the firmware to perform Auto Adjust and set the Bead Voltage.
NPD software requirements

This discussion assumes that the following firmware/software is installed: Table 70
Product 7890A GC Agilent GC ChemStation Agilent MSD ChemStation Agilent EZ Chrom Elite
Software requirements
Software/firmware revision A.01.08 or higher B.04.01 or higher G1701EA or higher 3.3.2 or higher
Software/firmware with numbers less than shown in the table can cause reduced bead lifetime. See the Agilent web site (www.agilent.com) for firmware and software updates.
NPD flows and general information

The NPD passes sample and carrier through a hydrogen/air plasma. A heated ceramic or glass source, called the bead, is just above the jet. The low hydrogen/air ratio cannot sustain a flame, minimizing hydrocarbon ionization, while the alkali ions on the bead surface facilitate ionization of nitrogen- or phosphorus- organic compounds. The output current is
Advanced User Guide
329
10 Detectors
proportional to the number of ions collected. It is sensed by an electrometer, converted to digital form, and sent to an output device.
H2 Makeup Air
Frit Valve
Frit Valve
Frit Valve
EPC Module
Vent PS Electrically heated bead
PS
PS
Restrictor
Restrictor
Restrictor
Column
NPD flow, temperature, and bead recommendations

Table 71
Gas or Setting
General operating values

Recommendation
Carrier gas (helium, hydrogen, nitrogen) Capillary, choose optimum flow based on column dimensions. Detector gases Hydrogen Ceramic bead 2 to 5 mL/min Blos bead 1 to 3 mL/min Ceramic bead 60 mL/min Blos bead 120 mL/min
Air
330
Advanced User Guide
Detectors
10
Table 71
Gas or Setting
General operating values (continued)

Recommendation Ceramic bead Nitrogen: 5 to 10 mL/min Helium: less than 5 mL/min Blos bead 1 to 20 mL/min
Capillary makeup (helium, nitrogen)
Temperature Default is 250 C; operating range is 150 C to 400 C. <150 C, the Adjust offset process will not start. 325 to 335 C is recommended. Detector temperature should be greater than the highest oven temperature. With higher detector temperatures, less bead heating voltage is required. Adjust offset Default is 30 pA, suggested operating range is 20 to 40 pA, and allowable range is 0 to 99.9 pA. 50 pA increases sensitivity but reduces bead life. Lower settings reduce sensitivity and increase bead life, but settings too low will result in solvent quenching. The time required for Adjust offset depends on the bead type and condition. Bead voltage Ceramic bead. Range is 0 to 4.095 V. Blos bead. Range is 0.5 to 1.1 V. Use Auto Adjust On, Dry Bead, and let the GC set the Bead Voltage for you.
Source gas pressures

Choose a flow, find a pressure, and set source pressure 10 psi (70 kPa) higher.
Advanced User Guide
331
10 Detectors
150 Air 100 Flow, mL/min 50 Nitrogen Helium
Pressure (psig) (kPa) 5 4
10 69
20 138
30 207
40 276
50 345
60 414
70 483
Hydrogen 3 Flow, mL/min 2 1
4 28
8 55
12 83
16 110
20 138
Temperature programming
The NPD is flow sensitive. If you are using temperature programming, in which the column flow resistance changes with temperature, set up the instrument as follows: Set the carrier gas in the Constant flow mode. Set detector makeup gas to Constant makeup. If you choose to work in the constant pressure mode, the makeup gas should be set in the Column +makeup=constant mode.
NPD required gas purity

Because of its high sensitivity, the NPD requires very pure (at least 99.9995%) gases. We strongly recommend that moisture and organics traps be used on the carrier gas and
332
Advanced User Guide
Detectors
10
all detector gases, including the detector hydrogen, air, and makeup gases. Do not use plastic (including Teflon) tubing, plastic- bodied traps, or O- ring seals.
Setting parameters for the NPD

Before operating the NPD, make sure that detector gases are connected, a column is installed, and the system is free of leaks. Set the oven temperature, inlet temperature, and column flow.
WA R N I N G
Make sure that a column is installed or the NPD column fitting is plugged before turning on the air or hydrogen. An explosion may occur if air and hydrogen are allowed to leak into the oven.
1 Select the bead (white ceramic, black ceramic, Blos). 2 Select the jet. 3 Install bead and jet as required. (See the Maintenance
Manual for details.)

4 Press [Config][Front Det] or [Config][Back Det]. 5 If you are using makeup gas, verify that the configured
makeup gas type is the same as that plumbed to your instrument. Change the gas type, if necessary. Nitrogen is recommended.
6 If the displayed Bead Type is incorrect, set the Bead Type
using the [Mode/Type] key.

7 Set Auto Adjust (On recommended). 8 Set Dry Bead (On recommended). 9 Press [Front Det] or [Back Det]. 10 Set the detector temperature. The recommended range is
325 to 335 C.
11 Enter a hydrogen flow (3.0 mL/min is recommended).
Turn the flow On.

12 Enter an air flow (60 is recommended for ceramic beads,
120 for Blos beads). Turn the flow On.

a If you are using packed columns, turn off makeup gas
and proceed to step 13.

b If your capillary column is defined, choose a flow
mode and set the makeup gas flow. For a column in the constant flow mode, choose Constant makeup. For a
Advanced User Guide
333
10 Detectors
column in the constant pressure mode, choose Column +makeup=constant.

c If your column is not defined, enter a makeup gas
flow. Only constant flow is available.

13 Monitor the offset adjustment process. a If Auto Adjust is On, the adjust offset process starts
automatically when the detector reaches setpoint. If Auto Adjust is Off, the Bead Voltage will gradually go to the last setpoint after the bead reaches setpoint temperature and the Dry Bead time has elapsed.
b If you need to set a new target offset, enter an Adjust
offset value. Adjust offset starts when the detector reaches setpoint.
c If Auto Adjust is Off, you can manually start the Adjust
offset process by scrolling to Adjust offset, then pressing [On/Yes].

d If your standard operating procedures require that you
set the bead voltage directly, see Setting NPD bead voltage manually (optional) on page 340.
Selecting an NPD bead type

Three beads are available: Table 72
Bead type White ceramic Black ceramic
NPD beads
Part number G1534-60570 5183-2007 Advantages Standard Durable, no phosphorus tailing Moisture resistant, long life Disadvantages Phosphorus tails Lower nitrogen sensitivity, about 40%
Blos bead
G3434-60806
334
Advanced User Guide
Detectors
10
Ceramic beads
Blos bead
Changing from a ceramic bead to a Blos bead

CAUTION The Blos bead is more delicate than the ceramic beads, and may be distorted during shipping. Before installing a Blos bead, verify that it is centered and adjust it if necessary.
When you turn the NPD off, the GC remembers the bead voltage used and applies that voltage when the detector is turned back on. If you have changed from a ceramic bead to a Blos bead, this voltage will be too high and may damage the new bead. To avoid this, reduce the voltage to the ceramic bead to 0.5 V before turning the detector off. When it restarts, the lower voltage will be applied.
Selecting an NPD jet

Open the oven door and locate the column connection fitting at the base of the detector. It will look like either a capillary optimized fitting or an adaptable fitting.
Capillary optimized fitting Adaptable fitting Detector fitting
Adapter
If you have an application that tends to clog the jet, select a jet with a wider tip id. When using packed columns in high column- bleed applications, the jet tends to clog with silicon dioxide.
Advanced User Guide
335
10 Detectors
For capillary optimized fittings, select one of the following from Table 73. Table 73
Figure 3 ID 1 2 3
Jets for capillary optimized fittings

Jet type Capillary with extended jet (recommended) Capillary High-temperature Part number G1534-80580 G1531-80560 G1531-80620 Jet tip id 0.29 mm (0.011 inch) 0.29 mm (0.011 inch) 0.47 mm (0.018 inch) Length 51.5 mm 43 mm 43 mm
51.5 mm 1 43 mm 2 43 mm 3 1 2 3
Figure 1
Capillary optimized NPD jets
For the adjustable NPD, select one of the following from Table 74. Table 74
Figure 4 ID 1 2 3 4
Jets for adaptable fittings

Jet type Capillary with extended jet (recommended) Capillary Capillary, high-temperature Packed Part number G1534-80590 19244-80560 19244-80620 18710-20119 Jet tip id 0.29 mm (0.11 inch) 0.29 mm (0.011 inch) 0.47 mm (0.018 inch) 0.46 mm (0.018 inch) Length 70.5 mm 61.5 mm 61.5 mm 63.6 mm
336
Advanced User Guide
Detectors
10
70.5 mm 1 61.5 mm 2 61.5 mm 3 63.6 mm 4 1 2 3 4
Figure 2
Adaptable NPD jets
To configure the NPD

In addition to the Ignore Ready and Makeup gas type, the NPD requires the following configuration settings. Scroll to each and enable/disable using [On/Yes] or [Off/No].
Auto Adjust Bead Recommended On. When On, the automatic adjust offset process starts when the bead reaches the temperature setpoint after having been turned off or cooled below 150 C. Auto adjust starts after Dry Bead hold time, if enabled. Auto Adjust Bead uses the adjust offset feature to protect the beadespecially new beadsby making sure that the desired offset is obtained with the lowest possible bead voltage. When Off, the bead voltage will rise as soon as the Dry Bead time elapses, or as soon as the temperature setpoint is reached if Dry Bead is off. Dry Bead Recommended On. When On, the bead temperature holds at 150 C for 5 minutes before continuing to the setpoint. This allows any condensation to evaporate and be swept out of the detector. Blos Bead If using a Blos bead, set to On. For ceramic beads, set to Off. The Blos Bead On setting restricts the allowable bead voltage to the range appropriate for this bead. Maximum Bead Voltage Display only. Shows the current maximum bead voltage for the configured bead type (4.095 V for ceramic beads, 1.1 V for the Blos bead).
Advanced User Guide
337
10 Detectors
Automatically adjusting NPD bead voltage

Agilent recommends using the Adjust offset feature to automatically determine the lowest bead voltage needed to give the desired response. When the detector is turned on, the temperature rises at a controlled rate. If Dry Bead is On, temperature holds at 150 C for 5 minutes to drive off moisture, then continues to the setpoint. If Dry Bead is Off, the temperature rises directly to the setpoint. When the temperature reaches the setpoint, the Bead Voltage gradually rises until it produces the desired output.
Adjust offset
When you enter a value here, or press [On/Yes] to use the stored value, detector gas flows turn on, the bead heats, and the bead voltage adjusts until Output is stable and equal to the entered value. There are five stages of Adjust offset.
Detector off When the detector is off, Adjust offset and Bead voltage are Off and initial Output is displayed. Detector ondetector temperature less than 150 C. When you enter an Adjust offset value or press [On], detector gases turn on and the display blinks the Temp not ready message. Detector onwaiting for oven and/or detector to reach temperature setpoint and equilibrium. If the oven or detector is not at setpoint, the display continues to blink the Temp not ready message. Detector onDry Bead On If Dry Bead is On, the temperature rise holds at 150 C for 5 minutes to remove moisture, then continues to the setpoint. Detector onduring adjust offset. When the detector and oven temperatures reach setpoint and equilibrate, the Adjust offset process begins. The bead voltage is slowly increased until the output is close to the Adjust offset value. The display blinks Detector Slewing.
338
Advanced User Guide
Detectors
10
Detector on and ready. When the Adjust offset value is reached, the Adjust offset line reads Done and displays the offset target setpoint. Your detector is on and ready. The display shows the actual Bead voltage.
Setting NPD adjust offset on the clock table

You can use the Clock table feature to begin Adjust offset at a specified time.
Aborting NPD adjust offset

Press [Delete] with the cursor on the Adjust offset line. This cancels the adjustment without turning off the detector gases and bead voltage.
Extending the NPD bead life

These actions, together with the automated heatup and adjust procedures, can extend ceramic bead life considerably. Use the lowest practical Adjust offset value. This will result in a lower Bead Voltage during operation. Run clean samples. Turn the bead off when not in use. Keep the detector temperature high (320 to 335 C). Turn the hydrogen flow off during solvent peaks and between runs.
Turning hydrogen off during a solvent peak

When using the NPD, the baseline shifts after a solvent peak and can take some time to stabilize, especially with chlorinated solvents. To minimize this effect, turn off the hydrogen flow during the solvent peak and turn it back on after the solvent elutes. With this technique, the baseline recovers to its original value in less than 30 seconds. This also extends the life of the bead. The hydrogen can be turned on and off automatically as part of a Run Table. See Run Time Programming on page 16.
Advanced User Guide
339
10 Detectors
Turning hydrogen off between runs

To extend bead life, turn off the hydrogen flow between runs. Leave all other flows and the detector temperature on. Turn on the hydrogen flow for the next run; the bead will ignite almost immediately. The process can be automated with Run Table entries.
Turning off the detector CAUTION If you turn Adjust offset [Off] at any time, the bead voltage, hydrogen, and air flows all turn off.
Setting the initial bead voltage for new beads

Before you turn on the bead for the first time, manually set its voltage to a safe value so that the new bead is not destroyed.
1 Make sure Adjust Offset is turned Off. 2 After the temperature stabilizes at setpoint, set the initial
Bead Voltage, depending on bead type: Blos bead: 0.0 V to 0.5 V Ceramic bead (white or black): 0.0 V to 2.0 V
Setting NPD bead voltage manually (optional)

Bead voltage shows the voltage used to heat the bead. It can be a value derived from the Adjust offset value, or can be entered as a setpoint. Entering a setpoint causes the voltage to change at 13 mV/second until it reaches the setpoint provided that the detector is at the temperature setpoint temperature is at least 150 C gas flows are on Dry Bead time, if On, has elapsed Bead voltage is also useful for small adjustments between runs. If you observe a baseline drift, you can enter a small, one- time change to compensate for the drift. If you are not using the recommended Adjust offset process, note that large voltage jumps reduce bead life. Use increments no greater than 0.05 V, spaced 10 seconds apart, until you reach the desired offset.
Detectors
10
New beads
After a new bead reaches the initial voltage, begin to increase the voltage value in 0.05 V increments until the bead ignites. Wait about 10 seconds between each voltage adjustment. Monitor the detector output. When the bead ignites, the output will rise suddenly, then decrease towards a more stable value. It is best to allow the NPD to remain in this state without further adjustment for about 24 hours. Then you may adjust the bead voltage in small increments (0.05 to 0.1 V) until reaching the desired offset. With a clean environment, clean gas supplies, and low bleed column, a typical offset may decrease 6- 12 pA during a 24 hour period. Typical voltages for new ceramic beads range from 2.5 to 3.7 volts. Higher values reduce bead life. Typical voltages for new Blos beads range from 0.5 to 1.0 V.
Advanced User Guide
341
10 Detectors
About the FPD

The sample burns in a hydrogen- rich flame, where some species are reduced and excited. The gas flow moves the excited species to a cooler emission zone above the flame where they decay and emit light. A narrow bandpass filter selects light unique to one species, while a shield prevents intense carbon emission from reaching the photomultiplier tube (PMT). The light strikes a photosensitive surface in the PMT where a light photon knocks loose an electron. The electron is amplified inside the PMT for an overall gain of up to a million.
H2 Makeup Air
Frit Valve
Frit Valve
Frit Valve PS
EPC Module Vent Emission Zone
PS
PS
Restrictor Wavelength filter Window
Restrictor
Restrictor
Column
The current from the PMT is amplified and digitized by the FPD electronics board. The signal is available either as a digital signal on the communications output or as a voltage signal on the analog output. The FPD should not be stored at temperatures above 50 C, based on the original manufacturers specifications for the PMT.
342
Advanced User Guide
Detectors
10
FPD linearity
Several mechanisms produce sulfur emission. The excited species is diatomic, so that emission intensity is approximately proportional to the square of the sulfur atom concentration. The excited species in the phosphorus mode is monatomic, leading to a linear relationship between emission intensity and atom concentration.
FPD Lit Offset

The default Lit Offset is 2.0 pA.
Starting Up and Shutting Down the FPD

The FPD creates a great deal of water vapor when the flame is on. This could condense in the vent tube on top of the detector and drop onto the flame, possibly extinguishing it. To avoid this, turn the heaters on, wait 20 minutes for the vent to heat up, and then ignite the flame. Water vapor will now make it over the top of the vent tube before condensing. For similar reasons, extinguish the flame before turning the heaters off.
FPD photomultiplier protection

The PMT is extremely sensitive to light. Always turn the PMT voltage off (which turns off the high voltage to the PMT) before removing the PMT housing or opening the emissions chamber. Failing to do this can destroy the PMT. Even with the PMT voltage off, protect the PMT from room light. Cap the housing when removed, place it end down to exclude light, reduce room light level before exposing the PMT, and so on. A brief exposure (always with the PMT voltage turned off) will not damage it but prolonged exposure will cause a gradual loss of sensitivity.
FPD optical filters

The filters are marked on the edge with the transmission wavelength. Each filter has a small arrow on its side which must point toward the PMT when installed. The sulfur filter is silvery on both sides and transmits at 393 nanometers.
10 Detectors
The phosphorus filter is yellow/green and transmits at 525 nanometers.
Inlet liners for use with the FPD

Compounds containing sulfur may adsorb on an inlet liner and degrade the GCs performance. Use deactivated, clean liners or a cool on- column inlet, which injects directly onto the column. For best results with splitless injection, use liner 5181- 3316.
FPD temperature considerations

The minimum detector temperature to prevent water condensation is 120 C. We recommend a temperature that is 25 C higher than the highest column temperature, but no higher than 250 C.
FPD gas purity

High- purity gases have a lower sulfur content. Standard purity gases have a higher sulfur content which impairs sulfur detection in the compound being studied. Instrument or Chromatographic grades work well. Agilent recommends using helium carrier, nitrogen makeup gas, and air with 99.9995% purity or better. Use carbon, oxygen, and moisture traps. Select traps to remove sulfur compounds from detector air and nitrogen gases. A helium getter is also recommended.
FPD gas flows

Table 75 gives the flows for the maximum sensitivity FPD flame, which is hydrogen- rich and oxygen- poor. Table 75 Recommended flows
Sulfur mode flows, mL/min Carrier (hydrogen, helium, nitrogen, argon) Packed columns Capillary columns Detector gases 10 to 60 1 to 5 10 to 60 1 to 5 Phosphorus mode flows, mL/min
344
Advanced User Guide
Detectors
10
Table 75
Recommended flows (continued)

Sulfur mode flows, mL/min Phosphorus mode flows, mL/min 75 100 60
Hydrogen Air Carrier + makeup
50 60 60
Helium, either as carrier or makeup gas, may cool the detector gases below the ignition temperature. We recommend using nitrogen rather than helium.
Lighting the FPD flame

Before trying to light the flame, have the detector at operating temperature. Removing the condensate tubing may help, but be sure to replace it before making runs. It is difficult to light the flame with the flows shown in Table 75, particularly in the sulfur mode. If the flame will not light with the sulfur mode flows shown, change to the phosphorus mode flows. After ignition, gradually reduce the flows to the sulfur values. Some experimentation will be needed. When either of the flame ignition methods in this section is used, the FPD automatically performs this sequence:
1 Turns all detector gasesair, hydrogen, makeupoff.
Carrier remains on.

2 Sets air flow to 200 mL/min. 3 Turns the glow plug ignitor on. 4 Ramps the hydrogen flow from 10 to 70 mL/min. 5 Resets the air flow to the air flow setpoint. 6 Resets the hydrogen flow to the hydrogen flow setpoint. 7 Turns the makeup gas on. 8 Compares the signal change with the Lit offset value. If the
change is greater than Lit offset, declares the flame on (lit). If it is less, declares the flame off (not lit). For this process to work, there must be enough air pressure to the pneumatics module to provide 200 mL/min flow. We recommend a supply pressure of 90 psi.
Advanced User Guide
345
10 Detectors
Manual ignition
1 Press [Front Det] or [Back Det]. 2 Scroll to Flame. Press [On/Yes]. The flame ignition
sequence begins.
Automatic ignition
If the FPD output with the flame on falls below the flame- off output plus the Lit offset value, this is interpreted as a flame- out condition. The FPD runs the flame ignition sequence to relight the flame. If this fails, it runs the sequence again. If the second attempt also fails, the detector shuts down all functions except temperature and makeup gas flow.
Setting parameters for the FPD

WA R N I N G Verify that a column is installed or the FPD fitting is plugged before turning on the air or hydrogen. An explosion may occur if air and hydrogen are allowed to leak into the oven.
1 Press [Front det] or [Back det]. 2 Set the detector temperature. It must be greater than
120 C for the flame to light.

3 Change the hydrogen flow rate, if desired. Press [Off/No]. 4 Change the air flow rate, if desired. Press [Off/No]. 5 If you are using packed columns, turn off the makeup gas
and proceed to step 7.

6 If you are using capillary columns: a Verify that makeup gas type is the same as that
plumbed to your instrument (next to Makeup in the parameter list). Change the gas type, if necessary.
b If your capillary column is defined, choose a flow
mode and set the makeup gas flow or combined flow.

c If your capillary column is not defined, enter a makeup
gas flow. Only constant flow is available.

7 Scroll to Flame and press [On/Yes]. This turns on the air
and hydrogen and initiates the ignition sequence. On ignition, the signal increases. Typical levels are 4 to 40 pA in sulfur mode, 10 to 70 pA in phosphorus mode. Verify that the flame is lit by holding a cold, shiny
Detectors
10
surface, such as a mirror or chrome- plated wrench, over the vent exit. Steady condensation indicates that the flame is lit.
Advanced User Guide
347
10 Detectors
348
Advanced User Guide
11 Valves
About Valves 350 The Valve Box 351 Heating the valves 351 Valve temperature programming 352 Configuring an Aux thermal zone 352 Valve Control 353 The valve drivers 353 The internal valve drivers 353 The external valve drivers 354 Valve Types 355 Configuring a Valve 356 Controlling a Valve 357 From the keyboard 357 From the run or clock time tables 357 Simple valve: column selection 357 Gas sampling valve 358 Multiposition stream selection valve with sampling valve 359
349
11 Valves
About Valves
Valves may be used to alter the usual inlet/column/detector flow path in the GC. Sampling valves can replace the inlet, switching valves can select columns, multiposition valves, used in conjunction with sampling valves, can perform the same functions for sample streams that an ALS performs for liquid samples.
350
Advanced User Guide
Valves
11
The Valve Box

The GC holds up to four valves in a heated valve box on top of the oven. The valve box is the preferred location for valves because it is a stable temperature zone, isolated from the column oven.
Back of chromatograph
Valve heater blocks
Valve box, cover removed
Figure 3
Diagram of valve locations on GC
Valves may also be mounted inside the column oven.
Heating the valves

The valve box contains two heated blocks, each with two valve mounting locations (shaded in Figure 3).a The middle hole on each block is used to pass tubing into the column oven. If two valves are used, mount them on the same block. This allows them to be heated using only one control channel (Aux Temp 1 or Aux Temp 2, depending on how the heaters are wired). With more than two valves, both channels must be used for heating the two blocks. Set them at the same temperature.
Advanced User Guide
351
11 Valves
Valve temperature programming

Most valve applications are isothermal; however, you can define three temperature ramps if desired. Press [Aux Temp #], then [1] or [2]. Program this ramp the same as an oven ramp. Refer to Setting the oven parameters for ramped temperature on page 292 for more information.
Configuring an Aux thermal zone

To configure a thermal Aux zone (1 or 2), press [Config][Aux Temp #], then [1] or [2]. Press [Mode/Type], then select the type of device to be controlled. Press [Enter].
352
Advanced User Guide
Valves
11
Valve Control
Valves can be controlled manually from the keyboard or as part of a clock or run time program. Note that only sampling valves automatically reset at the end of a run. Other valve types remain at the new position until activated again. For other valve types, you must include any desired resets in the program.
The valve drivers

A valve driver is the software and circuitry in the GC that controls a valve or related function. There are eight drivers known as Valve 1 through Valve 8. Table 76
Valve number 1, 2, 3, and 4 5 and 6 7 and 8
Valve drivers
Type Current source Current source Contact closure Volts 24 VDC 24 VDC 48 VDC or 48 VAC RMS Power or current 13 watts 100 mA Use Pneumatic valve control Relays and low-power devices Control an external current source
The internal valve drivers

Valve drivers 1 through 4 are usually used to control pneumatically operated valves mounted in the valve box. The wiring for these appears at a set of connectors inside the right cover of the GC. Pneumatically driven valves are controlled by solenoids mounted near the connectors that control the flow of air to the valve actuators.
Advanced User Guide
353
11 Valves
Keyboard Connector V1 or Connector V2 Run table or Connector V4 Clock table Internal valve drivers (1 through 4) Connector V3
There is no direct relationship between the location of a valve in the valve box and the driver that controls it. This depends on how the solenoids are wired and the actuators are plumbed. Manual valves must be switch by hand, and are heated or unheated.
The external valve drivers

Valve drivers 5 and 6 control a current that may be used to drive a relay or other low- power device. Valve drivers 7 and 8 switch a current from an external source. Electrical details are in Table 76 on page 353. These drivers, particularly Valve 7 and 8, may be used to control a motor driven multiposition valve for stream selection. All four of these drivers appear on the External Event connector on the back of the GC.
Keyboard or Run table or Clock table External valve drivers (5 through 8) Valve 5 (pin 1) and ground (pin 3 or 4) Valve 6 (pin 2) and ground (pin 3 or 4) Valve 7 (pin 5 and pin 6) Valve 8 (pin 7 and pin 8)
354
Advanced User Guide
Valves
11
Valve Types
There possible valve types are:
Sampling A two- position (load and inject) valve. In load position, an external sample stream flows through an attached (gas sampling) or internal (liquid sampling) loop and out to waste. In inject position, the filled sampling loop is inserted into the carrier gas stream. When the valve switches from Load to Inject, it starts a run if one is not already in progress. See the example on page 358. Switching A two- position valve with four, six, or more ports. These are general- purpose valves used for such tasks as column selection, column isolation, and many others. For an example of valve control, see page 359. Multiposition Also called a stream selection valve. It is usually used to select one from a number of gas streams and feed it to a sampling valve for analysis. It has a special actuator that advances the valve one position each time it is activated, or it may be motor driven. An example that combines a stream selection valve with a gas sampling valve is on page 359. Other
Could be anything. Self- explanatory.
Not installed
Advanced User Guide
355
11 Valves
Configuring a Valve
1 Press [Config]. Scroll to Valve #. 2 Enter the valve number and press [Enter]. The current
valve type is displayed.

3 To change the valve type, press [Mode/Type], select the
new valve type, and press [Enter].
356
Advanced User Guide
Valves
11
Controlling a Valve
From the keyboard
Valves (except multiposition valves) have two positions controlled by the [On] and [Off] keys. The keyboard commands for two- position valves are: [Valve #] <scroll to the valve> [On] stop and [Valve #] <scroll to the valve> [Off] other stop Rotates valve to the Rotates valve to one
From the run or clock time tables

The Valve On and Valve Off commands can be run time or clock time programmed. See Run Time Programming on page 16 and Clock Time Programming on page 19. If a valve is rotated by a run time program, it is not automatically returned to its initial position at the end of the run. You must program this reset operation yourself.
Simple valve: column selection

This is the plumbing for a single valve, configured as a switching valve, that selects one of two columns for analysis. It has no configuration parameters.
Front column
From inlet or sampling valve To detector
ON
Back column
OFF
The column is selected by pressing: [Valve #] <scroll to valve #> [On] (for the front column) or [Off] (for the back column).
Advanced User Guide
357
11 Valves
Use a run table entry to ensure that the valve is in the Off state between runs.
Gas sampling valve

If a valve is configured as a gas sampling valve, it starts a run automatically when it is switched to the Inject position. This can be done with a keyboard command or by a subsequence or clock table entry. You may have two gas sampling valves installed.
To column
Carrier in
LOAD position
INJECT position
Loop Sample in Sample out
Load position The loop is flushed with a stream of the sample gas. The column is flushed with carrier gas. Inject position The filled loop is inserted into the carrier gas stream. The sample is flushed onto the column. The run starts automatically.
Carrier gas may be provided by an (optional) auxiliary gas channel. To do this, configure the column and specify an Aux # channel as the inlet. The channel then becomes programmable with four operating modes. Sampling valves have two positions:
Load position The loop (external for gas sampling, internal for liquid sampling) is flushed with a stream of the sample. The column is flushed with carrier gas. Inject position The filled loop is inserted into the carrier gas stream. The sample is flushed onto the column. The run starts automatically.
The sampling valve control parameters are:
358
Advanced User Guide
Valves
11
Load time Time in minutes that the valve remains in the Load position before becoming ready. Inject time Time in minutes that the valve remains in the Inject position before returning to the Load position.
The sampling valve cycle is:
1 The sampling valve rotates to the Load position. Load time
begins. Valve is not ready.

2 Load time ends. The valve becomes ready. 3 If everything else is ready, the GC becomes ready. If
anything is not ready: If you are using Clock Table or sequence control, the GC waits until everything is ready, then executes the valve inject command. If you are not using Clock Table or sequence control, the valve injection can be made at any time from the keyboard.
4 The sampling valve rotates (keyboard command or
sequence control) to the Inject position. Inject time begins. The run begins.
5 Inject time ends. Return to step 1.
Multiposition stream selection valve with sampling valve

Several manufacturers provide multiposition stream selection valves that can be driven by valve drivers 1 through 4. Only one multiposition valve can be configured. If a valve is configured as a multiposition valve and has a BCD position output connected to the GC, the valve position can be selected directly.
Advanced User Guide
359
11 Valves
Sampling valve
Multiposition stream selection valve
Sample streams in Selected stream out
If the GC has one valve configured as a multiposition valve and another configured as a gas or liquid sampling valve, it assumes that they are to be used in series. This double configuration can be used to replace an automatic liquid sampler and sample tray in an analytical sequence. The multiposition valve becomes the sample tray; the sampling valve becomes the injector. Two configuration parameters provide mechanical and electrical compatibility with most multiposition valve actuators.
Switching time In seconds, is a delay between successive actuator movements. It allows time for the actuator mechanism to prepare for the next movement. Invert BCD Complements the BCD input; 1s become 0s and 0s become 1s. This accommodates coding convention differences among manufacturers.
360
Advanced User Guide
12 7683B Sampler
About the 7683B Sampler 362 Setting Parameters for the ALS 363 Solvent Saver 364 Sample tray setpoints 365 Storing setpoints 365
361
12 7683B Sampler
About the 7683B Sampler

The 7683B Automatic Liquid Sampler (ALS) is controlled by a sequence that specifies what samples are to be analyzed, where the sample vials are located in the sampler tray (if used), what methods are to be used for each sample, and possibly what to do after the last sample to clean out the column. See Creating Sequences on page 115 for more information on sequences.
Hardware
Consult the 7683B for all mechanical details, such as installing/removing the tray, injectors, bar code reader, syringes, and so on. Follow the instructions for the 6890N GC.
Software
The new 7890A parameters are described in this chapter. Follow these instructions for all non- mechanical operations.
362
Advanced User Guide
7683B Sampler
12
Setting Parameters for the ALS

Pressing either of the injector keys allows you to edit injector control setpoints, such as injection volumes, sample and solvent washes, etc. To edit the injector setpoints:
1 Press [Front Injector] or [Back Injector]. 2 Scroll to the desired setpoint. 3 Enter a setpoint value, or turn the setpoint On or Off. 4 Press [Mode/Type] to make selections for syringe size and
syringe plunger speed.
Injection volume Sample volume to be injected. Press [Mode/Type] to select. The available volumes depend on the syringe size configured.
The selections represent 2%, 10%, 20%, 30%, 40%, and 50% of syringe size. Turn the injection volume Off to disable the injector.
Viscosity delay (0-7 seconds) How long the plunger pauses at the top of the pump and injection strokes. For viscous samples, the pause allows the sample to flow into the vacuum created in the syringe. Inject Dispense Speed The speed of the syringe plunger during injection. Enables you to reduce the average speed of the plunger. Press [Mode/Type] to see the choices. The plunger speed during the pump and waste dispensing does not change. Sample pumps (0-15) How many times the syringe plunger is moved up and down with the needle in the sample to expel air bubbles and improve reproducibility. Sample washes (0-15) How many times the syringe is rinsed with sample before the injection. The wash volume is set by the Solvent Saver setting. Solvent A post washes (0-15) How many times the syringe is washed with solvent A after injection. Solvent A pre washes (0-15) How many times the syringe is washed with solvent A before the sample washes.
Advanced User Guide
363
12 7683B Sampler
Solvent B post washes (0-15) How many times the syringe is washed with solvent B after any solvent A washes. Solvent B pre washes (0-15) How many times the syringe is washed with solvent B after any solvent A prewashes and before the sample washes. Solvent B wash volume The percent of the syringe volume to be used for solvent B washes. Sample Draw Speed Speed of the syringe plunger when drawing in sample. Sample Disp Speed Speed of the syringe plunger when dispensing sample. Solvent Draw Speed Speed of the syringe plunger when drawing in solvent. Solvent Disp Speed Speed of the syringe plunger when dispensing solvent. Pre dwell time (0-1) How long, in minutes, the needle remains in the inlet before the injection. Post dwell time (0-1) How long, in minutes, the needle remains in the inlet after injection. Sample offset (-2 to 30, Off) Sets variable sampling depth. Injection Reps (1-99) How many times the injection and analysis should be repeated from each vial. Injection Delay Time between multiple injections. Availability depends on the inlet type.
Solvent Saver
If you enter a non- zero value for any of the solvent or sample washes, the GC will ask for the wash volume. The default is 80% of the syringe volume. Press [Mode/Type] to see the other choices. This function allows you to conserve solvent during the washes.
364
Advanced User Guide
7683B Sampler
12
Sample tray setpoints

The sample tray delivers sample vials to the front and rear injectors according to the defined sequence parameters. There is a separate set of sequence parameters for each injector. The sample tray delivers vials to the front injector before the rear injector. Stored sequences and bar code configurations can be used to tell the sample tray where to deliver and retrieve sample vials.
Enable bar code
Turns the bar code reader on or off.
1 Press [Sample tray] to access the sample tray and bar code
reader setpoints.
2 Press [On] or [Off] to enable or disable the tray. 3 Press [On] or [Off] to enable or disable the bar code
reader.
Storing setpoints
After setting up injector setpoints, sample tray setpoints and bar code reader configurations, store them as part of a method by following the procedures in To store a method from the keypad. This method becomes a part of the sequence used to run the samples.
Advanced User Guide
365
12 7683B Sampler
366
Advanced User Guide
13 Cables
About Cables and Back Panel Connectors 368 Back panel connectors 368 Sampler connectors 368 The AUX connector 368 Signal connectors 369 REMOTE connector 369 EVENT connector 369 BCD input connector 369 RS-232 connector 369 LAN connector 369 Using the Remote Start/Stop cable 370 Cable Diagrams 375 Analog cable, general use 375 Remote start/stop cable 375 BCD cable 376 External event cable 377
367
13 Cables
About Cables and Back Panel Connectors

Some parts of an analysis system are connected to the GC by cables. These cables and the back panel connectors to which they connect are described in this section.
Back panel connectors

These are the connectors on the back panel of the GC:
SAMPLER 1 SAMPLER 2 TRAY AUX
SIG 1 SIG 2
REMOTE
RS-232
EVENT BCD LAN
Sampler connectors
If using an ALS, connect to the GC using the following connectors:
SAMPLER 1 An injector, usually the front injector. (For 7693A, the configuration does not matter. For a the 7683, typically configured as INJ1.) SAMPLER 2 A second injector, usually the back injector. (For 7693A, the configuration does not matter. For a the 7683, typically configured as INJ2.) TRAY
The sample tray and (optional) barcode reader.
The AUX connector

This connector is reserved for future development.
368
Advanced User Guide
Cables
13
Signal connectors
SIG1 and SIG2 are for the two analog output signals.
REMOTE connector
Provides a port to remotely start and stop other instruments. A maximum of 10 instruments can be synchronized using this connector. See Using the Remote Start/Stop cable on page 370 for more detail.
EVENT connector
This connector provides two passive contact closures and two 24- volt outputs for controlling external devices. The outputs are controlled by valve drivers 5 through 8.
BCD input connector

This connector provides two control relays and a BCD input for a stream selection valve.
CAUTION
This connector is similar to the EVENT connector. Plugging a non BCD cable into the BCD connector can damage the GC.
RS-232 connector
This connector is reserved for future development.
LAN connector
Standard Local Area Network connector, for communication with data systems and other devices.
Advanced User Guide
369
13 Cables
Using the Remote Start/Stop cable

Remote start/stop is used to synchronize two or more instruments. For example, you might connect an integrator and the GC so that the [Start]/[Stop] buttons on either instrument control both of them. You can synchronize a maximum of ten instruments using Remote cables.
Connecting Agilent products

If connecting two Agilent products with Remote cables, the sending and receiving circuits will be compatiblejust plug in both ends of the cable.
Connecting non-Agilent products

If connecting to a non- Agilent product, the following paragraphs contain information you will need to ensure compatibility.
APG Remote signal electrical specifications

The APG signals are a modified open collector type. The signal levels are generally TTL levels (low voltage is logic zero, high voltage is logic one) but the open circuit voltage will be between 2.5 and 3.7 Volts. The typical voltage is 3 Volts. A voltage over 2.2 volts will be interpreted as a high logic state while a voltage below 0.4 volts will be interpreted as a low logic state. These levels provide some margin over the specifications of the devices used. The pull- up resistance, connected to the open- circuit voltage, is in the range of about 1K ohms to 1.5K ohms. For a logic- low state, for a single device on the bus, the minimum current you must be able to sink is 3.3 milliamps. Since devices are connected in parallel, when you have multiple devices this minimum current must be multiplied by the number of devices attached on the bus. The maximum voltage for a low- input state = 0.4V. The bus is passively pulled high. Leakage current out of a port must be less than 0.2 milliamps to keep the voltage from being pulled lower than 2.2 volts. Higher leakage current may cause the state to be interpreted as a low. Over- voltage protection - APG Remote connections are clamped by a zener diode to 5.6 Volts. Exceeding this voltage will damage the circuit (main board).
370
Advanced User Guide
Cables
13
APG Remote - Suggested drive circuits

A signal on the APG bus may be driven by another APG device or by one of the following circuits: A relay, with one side connected to ground, when closed will set a logic- low state. An NPN transistor, with the emitter connected to ground and the collector connected to the signal line will set a logic- low state if proper base current is supplied. An open- collector logic gate will perform this same function. A low- side drive IC will also work, but Darlington- type drivers should be avoided as they will not meet the low- side voltage requirement of less than 0.4V
APG Remote connector
Pin 1 2 1 3 6 9 4 5 6 7 8 9
Function Digital ground Prepare Start Start relay Start relay not used Ready Stop not used
Logic
LOW true LOW true (input)
HIGH true (output) LOW true
APG Remote signal descriptions

Prepare (Low True) Request to prepare for analysis. Receiver is any module performing pre- analysis activities. For example, shorting pin 2 to ground will put the GC into Prep Run state. This is useful for Splitless Mode to prepare the inlet for injection or when using the Gas Saver. This function is not needed by Agilent autosampler systems. Ready (High True) If The Ready Line is high (> 2.2 VDC) then the system is ready for next analysis. Receiver is any sequence controller.
Advanced User Guide
371
13 Cables
Start (Low True) Request to start run/timetable. Receiver is any module performing runtime- controlled activities. The 7890 GC requires a pulse duration of at least 500 micro- seconds to sense a start from an external device. Start Relay (Contact Closure) A 120 millisecond contact closure used as an isolated output to start another device that is not compatible or connected with APG Remote pin 3. Stop (Low True) Request to reach system ready state as soon as possible (for example, stop run, abort or finish, and stop injection). Receiver is any module performing runtime- controlled activities. Normally this line is not connected, if the GC oven program is used to control the method Stop time.
APG Remote timing diagram

Runtime elapsed/Start Not Ready during Prep Injection cycle started
Request for Prepare
Waiting for Ready
Waiting for Ready
Start Requested
Injection/Start
System Ready
System Ready
Prepare
H L H L H L H H H L
Start Stop
Ready
372
System Ready
Postrun
Run
Advanced User Guide
Cables
13
Connecting Cables
Connect a GC to an Agilent data system computer using LAN communications using a LAN cable. See Figure 4 below.
LAN hub/switch Crossover LAN cable 5183-4648 LAN cable 8121-0940 LAN cable 8121-0940 Computer Computer
GC
GC
Figure 4
Connecting the GC and computer with a hub/switch (shown at left) or a crossover cable (shown at right).
Table 77
Typical IP addresses for an isolated LAN

GC Computer
IP address Subnet mask
10.1.1.101 255.255.255.0
10.1.1.100 255.255.255.0
A single communications LAN cable is supplied with the GC. The hub and other cables must be ordered separately, if needed. See Table 77 and Table 78 for cabling requirements for other configurations.
Table 78 Cabling requirements
Required Cable(s) Part number
7890A GC connected to:
7693A Automatic Liquid Sampler 7683 Automatic Liquid Sampler G1289B/G1290B Headspace Sampler 7695 Purge and Trap Sampler
Injector cable or tray cable Injector cable is integral Tray cable Remote, 9-pin male/6-pin connector Remote, 25-pin male/9-pin male
G4514-60610
G2614-60610 G1530-60930 G1500-60820
Advanced User Guide
373
13 Cables
Table 78
Cabling requirements (continued)

Required Cable(s) Part number
7890A GC connected to:
CTC automatic sampler 3395B/3396C Integrator Non-Agilent Integrator Mass Selective Detector Non-Agilent data system Non-Agilent instrument, unspecified Stream selection valves Gas sampling valves LAN
Remote, Remote, 9 pin/15 pin Analog, 2 m, 6 pin General purpose analog signal cable 2 m, 6 pin Remote, 2-m, 9-pin male/9-pin male General use remote, 9-pin male/spade lugs (various lengths) External event, 8 pin/spade lugs See documentation accompanying the valve Cable, networking CAT 5, 8121-0940 25 feet Cable, LAN, crossover 5183-4648 03396-61010 G1530-60570 G1530-60560
G1530-60930 35900-60670 (2 m), 35900-60920 (5 m), 35900-60930 (0.5 m) G1530-60590
Table 79 Instrument 1 Modem
Cabling for other instruments in a 7890A system Instrument 2 PC Type of cable Modem, 9-pin female/9-pin male, or Modem, 9-pin female/25-pin male Splitter ("Y") cable for remote, 1 male and 2 female connectors Part no. G1530-61120, or 24540-80012 G1530-61200
Mass Selective Detector
Purge & Trap or Headspace sampler
Splitter ("H") cable for 35900-60800 APG remote, 2 male and 2 female connectors
374
Advanced User Guide
Cables
13
Cable Diagrams
Analog cable, general use
Connector 1
Connector 2
The pin assignments for the general use analog out cable are listed in Table 80.
Table 80 Connector 1 1 2 3 4 6 Shell Analog cable, general use, output connections Connector 2, wire color Brown or violet White Red Black Blue Orange Signal Not used 0 to 1 V, 0 to 10 V () Not used 1 V (+) 10 V (+) Ground
Remote start/stop cable
Connector 1 Connector 2
The pin assignments for the remote start/stop cable are listed in Table 81.
Advanced User Guide
375
13 Cables
Table 81
Remote start/stop cable connections Connector 2, wire color Black White Red Green Brown Blue Orange Yellow Violet Signal Digital ground Prepare (low tone) Start (low tone) Start relay (closed during start) Start relay (closed during start) Open circuit Ready (high true input) Stop (low tone) Open circuit
Connector 1, 9-pin male 1 2 3 4 5 6 7 8 9
BCD cable
The BCD connector has eight passive inputs that sense total binary- coded decimal levels. The pin assignments for this connector are listed in Table 82.
Table 82 Pin 1 2 3 4 5 6 7 8 Shield BCD input connections Function Relay Relay LS digit 0 LS digit 1 LS digit 2 LS digit 3 MS digit 0 Ground Chassis ground Maximum rating 48 V AC/DC, 250 mA 48 V AC/DC, 250 mA
376
Advanced User Guide
Cables
13
External event cable

6 3 1 4 7 8 5 2
Connector 1
Connector 2
Two passive relay contact closures and two 24- volt control outputs are provided. Devices connected to the passive contact closures must be connected to their own power sources. The pin assignments for this cable are listed in Table 83.
Table 83 External events cable Signal name Maximum rating Connector 2, wire color Controlled by valve #
Connector 1 pin 24 volts output 1 2 3 4
24 V output 1 24 V output 1 Ground Ground
75 mA 75 mA
Yellow Black Red White
5 6
Relay contact closures (normally open) 5 6 7 8 Closure 1 Closure 1 Closure 2 Closure 2 48 V AC/DC, 250 mA 48 V AC/DC, 250 mA Orange Green Brown or violet Blue 7 7 8 8
Advanced User Guide
377
13 Cables
378
Advanced User Guide
14 GC Output Signals
About Signals 380 Signal Types 381 Value 381 Analog Signals 383 Analog zero 383 Analog range 383 Analog data rates 384 Selecting fast peaks (analog output) 385 Digital Signals 386 Digital zero 386 Baseline level shifts 386 Agilent data systems 387 Column Compensation 390 Creating a column compensation profile 391 Making a run using analog output column compensation 391 Plotting a stored column compensation profile 392 Test Plot 393
379
About Signals
Signal is the GC output to a data handling device, analog or digital. It can be a detector output or the output from flow, temperature, or pressure sensors. Two signal output channels are provided. Signal output can be either analog or digital, depending on your data handling device. Analog output is available at either of two speeds, suitable to peaks with minimum widths of 0.004 minutes (fast data rate) or 0.01 minutes (normal rate). Analog output ranges are 0 to 1 V, 0 to 10 V, and 0 to 1 mV. Digital output rates are set by your Agilent data system, such as ChemStation or EZChrom.
380
Advanced User Guide
GC Output Signals
14
Signal Types
When assigning detector signals, use the [Mode/Type] key and choose from the Signal Type parameter list, or press a key or combination of keys. [Front], [Back], [], and [Column Comp] will work, alone or in combination. For example, press [Back] for back detector or [Back][][Front] for back detector minus front detector. The menu choices for signal subtraction (Front - Back and Back Front) only appear if the front and back detectors are of the same type. The nondetector signals are test plot, thermal, pneumatic, and diagnostic. Access them by pressing [Mode/Type]. Diagnostic signals are for use by your service representative and are not described in detail here. Signal type can be programmed as a run time event.
Value
Value on the signal parameter list is the same as Output on the detector parameter list if your signal type is Front or Back. If you are subtracting one signal from another (as in Front Back), the signal Value will be the difference. You cannot enter a setpoint for Value. A conversion factor may be involved when interpreting Valuefor example, one FID unit is one picoamp; one uECD unit is 1 Hz. The units for detector and other signals are listed below. Table 84
Signal type Detector: FID, NPD FPD TCD ECD 1.0 pA (1.0 10-12 A) 150 pA (150 10-12 A) 25 mV (2.5 10-5 V) 1 Hz
Signal conversions
1 display unit is equivalent to:
Analog input board (use to connect the 15 V GC to non-Agilent detector) Nondetector: Thermal 1 C
Advanced User Guide
381
Table 84
Signal type Pneumatic: Flow Pressure Diagnostic
Signal conversions (continued)

1 display unit is equivalent to: 1 mL/min 1 pressure unit (psi, bar, or kPa) Mixed, some unscaled
382
Advanced User Guide
GC Output Signals
14
Analog Signals
If you use an analog recorder, you may need to adjust the signal to make it more usable. Zero and Range in the Signal parameter list do this.
Analog zero
Zero Subtracts value entered from baseline. Press [On/Yes] to set to current Value or [Off/No] to cancel.
This is used to correct baseline elevation or offsets. A common application is to correct a baseline shift that occurs as the result of a valve operation. After zeroing, the analog output signal is equal to the Value line of the parameter list minus the Zero setpoint. Zero can be programmed as a run time event. For details, see Run Time Programming on page 16.
1 Verify that the detector is on and in a ready state. 2 Press [Analog Out 1] or [Analog Out 2]. 3 Scroll to Zero. 4 Press [On/Yes] to set Zero at the current signal value,
or Enter a number between - 500000 and +500000. A value smaller than the current Zero shifts baseline up.
Analog range
Range Scales data coming from the detector
Range is also referred to as gain, scaling, or sizing. It sizes the data coming from the detector to the analog signal circuits to avoid overloading the circuits (clamping). Range scales all analog signals. If a chromatogram looks like A or B in the next figure, the data needs to be scaled (as in C) so that all peaks are visible on the paper. Valid setpoints are from 0 to 13 and represent 20 (=1) to 213 (=8192). Changing a setpoint by 1 changes the height of the chromatogram by a factor of 2. The following chromatograms illustrate this. Use the smallest possible value to minimize integration error.
Advanced User Guide
383
A: Range = 0
B: Range = 3
C: Range = 1
There are limits to usable range settings for some detectors. The table lists the valid range setpoints by detector. Table 85
Detector FID NPD FPD TCD ECD Analog input
Range limits
Usable range settings (2x) 0 to 13 0 to 13 0 to 13 0 to 6 0 to 6 0 to 7
Range may be run time programmed. See Run Time Programming on page 16 for details.
Analog data rates

Your integrator or recorder must be fast enough to process data coming from the GC. If it cannot keep up with the GC, the data may be damaged. This usually shows up as broadened peaks and loss of resolution. Speed is measured in terms of bandwidth. Your recorder or integrator should have a bandwidth twice that of the signal you are measuring. The GC allows you to operate at two speeds. The faster speed allows minimum peak widths of 0.004 minutes (8 Hz bandwidth), while the standard speed allows minimum peak widths of 0.01 minutes (1.6 Hz bandwidth). If you use the fast peaks feature, your integrator should operate at around 15 Hz.
GC Output Signals
14
Selecting fast peaks (analog output)

1 Press [Config][Analog 1] or [Config][Analog 2]. 2 Scroll to Fast peaks and press [On].
Agilent does not recommend using Fast peaks with a thermal conductivity detector. Since the gas streams switch at 5 Hz, the gain in peak width is offset by increased noise.
Advanced User Guide
385
Digital Signals
The GC outputs digital signals only to an Agilent data system. The following discussions describe features that impact the data sent to data systems, not the analog data available to integrators.
Digital zero
Digital signal outputs respond to the Zero command by subtracting the signal level at the time of the command from all future values.
Baseline level shifts

Some run time operations, such as changing signal assignment or switching a valve, can produce large changes in the signal baseline position. This can complicate signal processing by external devices. The GC provides two run table commands to minimize such problems with digital outputsee Run Time Programming on page 16.
Store signal value the command.
Saves the value of the signal at the time of
Signal zero value Creates a new zero by subtracting the stored value from the current value of the signal and applies this zero to all future values.
When these commands surround a baseline- shifting command, the effect is to bring the new baseline to the previous level, as shown in the next figure. The Store signal value event must occur before the event that shifts the baseline, and the Signal zero value event must occur after the baseline has stabilized at the shifted level.
386
Advanced User Guide
GC Output Signals
14
No correction
Baseline level change
Baseline shifting event occurs
Run time correction
3. Sig zero - val event occurs
2. Baseline shifting event occurs 1. Store signal value event occurs
Agilent data systems

The GC can process data at various data rates, each corresponding to a minimum peak width. The table shows the effect of data rate selection. Table 86
Data rate, Hz 500 200 100 50 20 10 5 2
EZChrom Elite/ChemStation data processing

Minimum peak width, minutes 0.0001 0.001 0.002 0.004 0.01 0.02 0.04 0.1 Relative noise 5 3.1 2.2 1.6 1 0.7 0.5 0.3 All types to Detector FID FID FID/FPD/NPD only Column type Narrow-bore, 0.05 mm Narrow-bore, 0.05 mm Capillary
Advanced User Guide
387
Table 86
Data rate, Hz 1 0.5 0.2 0.1
EZChrom Elite/ChemStation data processing (continued)

Minimum peak width, minutes 0.2 0.4 1.0 2.0 Relative noise 0.22 0.16 0.10 0.07 Slow packed Detector Column type
You cannot change the data rate during a run. You will see higher relative noise at the faster sampling rates. Doubling the data rate can double peak height while the relative noise increases by 40%. Although noise increases, the signal- to- noise ratio is better at the faster rates. This benefit only occurs if the original rate was too low, leading to peak broadening and reduced resolution. We suggest that rates be chosen so that the product of data rate and peak width in seconds is about 10 to 20. The figure shows the relationship between relative noise and data rates. Noise decreases as the data rate decreases until you get to data rates of around 5 Hz. As the sampling rate slows, other factors such as thermal noise increase noise levels.
Relative noise level
Excess noise (due to flow, oven temperature, detector block temperatures, etc.)
Faster data rates
Slower data rates
388
Advanced User Guide
GC Output Signals
14
Zero Init Data Files

This feature applies to digital output only, and is mainly intended for non- Agilent data systems. It may help systems that have trouble with non- zero baseline output. When you turn it On, the GC immediately begins to subtract the current detector output value(s) from any future values. For example, if you turn it on when the output is 20 pA, the GC subtracts 20 pA from the digital output until you turn Zero Init Data Files Off. You will not see any change in the GC display, but you will see the change in the online plot available in the data system.
Advanced User Guide
389
Column Compensation
In temperature programmed analysis, bleed from the column increases as the oven temperature rises. This causes a rising baseline which makes peak detection and integration more difficult. Column compensation corrects for this baseline rise. A column compensation run is made with no sample injected. The GC collects an array of data points from all 4 detectors, whether installed, off, or working. If a detector is not installed or is turned off, that part of the array is filled with zeros. One array (Column compensation 1) can be created for analog signals. Two independent arrays (Column compensation 1 and 2) can be created for digital signals. Each array defines a set of curves, one for each detector, that can be subtracted from the real run to produce a flat baseline. The next figure illustrates the concept.
Chromatogram with rising baseline Blank column compensation profile Chromatogram with column compensation
All conditions must be identical in the column compensation run and the real run. The same detector and column must be used, operating under the same temperature and gas flow conditions.
390
Advanced User Guide
GC Output Signals
14
Creating a column compensation profile

1 Set up the instrument for a run. 2 Make a blank run to verify that the baseline is clean. This
is particularly important for new conditions or if the GC has been idle for several hours.
3 Press [Column Comp]. 4 Select Col comp 1 or Col comp 2 (these are the two arrays). 5 Select Start compensation run and press [Enter]. 6 If the run is successful, the first line of the parameter list
will say Data ok, and a time and date will appear at the bottom.
Making a run using analog output column compensation

1 Set the chromatographic conditions. They must be
identical to those in the stored column compensation run except that Final time in the last ramp of the oven program can be longer or shorter.
2 Press [Analog Out 1] or [Analog Out 2]. 3 Scroll to Type and press [Mode/Type]. 4 The choices for an analog signal are:
Front detector Back detector Front - column comp 1 Front column compensation 1 Back column compensation 1 Aux 1 column compensation 1 Aux 2 column compensation 1 Test plot
5 Choose an option from the list. 6 Enter setpoints for Zero and Range, if applicable. 7 Start your run.
Making a run using digital output column compensation

1 Set each detector output separately. 2 Press [Config][Detector name]. Scroll to Signal and press
[Mode/Type]. Select from: No Column Compensation Detector - ColComp 1 Detector - ColComp 2

This changes the digital output. You cannot get both compensated and uncompensated digital data from the same detector at the same time. However, it does not affect the analog output.
Plotting a stored column compensation profile

1 Press [Analog Out 1] or [Analog Out 2]. 2 Scroll to Type: and press [Mode/Type]. 3 Select the profile to be plotted. 4 Press [Start].
392
Advanced User Guide
GC Output Signals
14
Test Plot
Test plot is an internally generated chromatogram that can be assigned to a signal output channel. It consists of three baseline- resolved, repeating peaks. The area of the largest is approximately 1 Volt- sec, the middle one is 0.1 times the largest, and the smallest is 0.01 times the largest.
Test plot can be used to verify the operation of external data processing devices without having to perform repeated chromatographic runs. It may also be used as a stable signal to compare the results from different data processing devices. To use the Test Plot:
1 Press [Analog Out 1] or [Analog Out 2]. 2 Scroll to Type: and press [Mode/Type]. 3 Choose Test Plot. 4 Press [Start]. The plot will repeat until you press [Stop].
Test Plot is the default choice for the analog outputs.
Advanced User Guide
393
394
Advanced User Guide
15 Miscellaneous Topics
Auxiliary Devices 396 About Auxiliary Pressure Control 396 About Aux Thermal Zone Control 397 About Auxiliary Device Contacts 397 About the 24V Auxiliary Device Power Supply 397 About Auxiliary Columns 397 About Auxiliary Detectors 398 To Use the Stopwatch 399 Service Mode 400 Service Reminders 400
395
Auxiliary Devices
About Auxiliary Pressure Control
Pressure units
There are two common ways of expressing gas pressures:
psia
Absolute pressure, measured relative to vacuum.
psig Gauge pressure, measured relative to atmospheric pressure. This name is used because most pressure gauges have one side of the sensing element exposed to the atmosphere.
The two measurements are related by: psia = psig + atmospheric pressure
Two-channel pressure control module (PCM)

The PCM has two different channels. Channel 1 may be either flow or pressure controlled and may be flow/pressure programmed. It is essentially identical to the packed column inlet flow module (see About the Multimode Inlet on page 191). Channel 2 is pressure only, but may be used in either a forward- or backpressure mode by changing connections. Both channels are controlled by the same parameter list. The first two lines are for channel 1; the remaining lines are for channel 2. The forward- pressure mode requires the user to supply a downstream flow resistance, possibly a frit. The backpressure mode is most useful with gas sampling valves. By connecting the sample exit line from the valve to the vent fitting of the PCM, pressure in the sample loop can be controlled.
Three-channel auxiliary pressure controller (Aux PCM)

All channels are 3- ramp programmable. Up to three modules may be installed, for a total of 9 pressure- regulated channels.
396
Advanced User Guide
15
Setting parameters for auxiliary pressure control

1 Press [Aux EPC #] and scroll to the channel you wish to
control. Press [Enter].

2 Scroll to Initial pressure. Enter a value and press [Enter]. 3 If desired, enter a pressure program using the time and
rate functions.
4 Press [On/Yes] to apply Initial pressure and start the
program.
About Aux Thermal Zone Control

There can be up to 3 aux thermal controlled zones. These zones are 3- ramp programmable. Run time events may be used to schedule specific temperatures during the run.
Setting parameters for the aux thermal zone control

1 Press [Aux Temp #] and scroll to the zone you wish to
control. Press [Enter].

2 Scroll to Temperature. Enter a value and press [Enter]. 3 Scroll to Initial time. Enter a value and press [Enter]. 4 Scroll to Rate 1. Enter 0 to end the program here or a
positive value to create a temperature program.
About Auxiliary Device Contacts

These contacts are controlled by the external valve drivers. See The external valve drivers on page 354.
About the 24V Auxiliary Device Power Supply

This is controlled by the external valve drivers. See The external valve drivers on page 354.
About Auxiliary Columns

Defines up to 6 columns (includes Col 1 and Col 2).
1 Press [Config][Aux Col #] and enter a column number. Press
[Enter].
2 Define/configure the column. See Column # on page 32
for details.
Advanced User Guide
397
About Auxiliary Detectors

The GC supports up to two auxiliary detectors in addition to the Front and Back detectors that mount on the top of the oven.
Aux Det # 1 This can only be a TCD, and mounts in a carrier on the left side of the oven together with its flow module. Aux Det # 2 This can only be an analog input board (AIB). It is used to receive and process data from a non- Agilent detector or other source.
398
Advanced User Guide
15
To Use the Stopwatch

In the stopwatch mode, both the time (to 0.1 second) and reciprocal time (to 0.01 min- 1) are displayed. The stopwatch is useful when measuring flows with a bubble flowmeter.
1 Press [Time] and scroll to the time = line. 2 Press [Enter] to start the stopwatch. 3 Press [Enter] again to stop. 4 Press [Clear] to set to zero.
You can access other functions while the stopwatch is running. Press [Time] again to view the stopwatch display.
Advanced User Guide
399
Service Mode
The [Service Mode] key presents the Service Reminders and other functions.
Service Reminders
Internal counters
This is a set of 12 counters that monitor the use of various items on the GC, such as syringes, septa, and columns. These counters only count runs and their definitions are fixed. You can set limits for each item; when a limit is reached, the Service Due light on the status board comes on. Examine the limits to identify the item that has reached its limit. You may enter a limit for each item, reset a count to 0 by pressing [Off/No], or disable a counter by entering a limit of 0.
Advanced counters
The GC provides storage for 64 advanced counters. They each have two thresholds, and the actions based on these counters can be: do nothing, turn on the Service Due light, or light the Service Due light and go Not ready. Advanced counters are not accessible through the GC keyboard, except for the Disable Advanced Counters function of the Service Reminders. If they are not disabled, they continue to count, and continue to act on the set thresholds. This could cause the GC to become Not ready. Since the advanced counters cannot be reset or manipulated without the Agilent G4600AA Lab Advisor software. Disable Advanced Counters is provided so that they can be turned off from the GC keyboard by someone who does not wish to use them, the Lab Advisor software, or an Agilent data system. These users should disable the advanced counters from the keypad to avoid possible problems. Counters can be individually enabled (count or dont count), individually reset (start over), and individually set as counting elapsed seconds or runs. They can be assigned arbitrary meanings, allowing you to set up counters for equipment of your choice.
400
Advanced User Guide
15
Each counter has an ID that can be associated with a concept, such as front inlet gold seal, and can count the number of elapsed runs or seconds since the last reset, from which one can infer the gold- seals in- service time or count. A ChemStation can enable or disable individual counters in association with a method, so that only the counters for things used by the method advance.
Other functions
These are for use by trained Agilent personnel. They are described in the Service Manual.
Advanced User Guide
401
402
Advanced User Guide

7890A Manual

Enviado por

Dados do documento

Descrição original:

Direitos autorais

Formatos disponíveis

Compartilhar este documento

Compartilhar ou incorporar documento

Opções de compartilhamento

Você considera este documento útil?

Este conteúdo é inapropriado?

Direitos autorais:

Formatos disponíveis

7890A Manual

Enviado por

Direitos autorais:

Formatos disponíveis

Agilent 7890A Gas Chromatograph

Advanced User Guide

Safety Notices CAUTION

Manual Part Number

Advanced User Guide

Advanced User Guide

Methods and Sequences

Advanced User Guide

Checking for Leaks

To Check for External Leaks To Check for GC Leaks 125

To Perform a VI Pressure Decay Test

Flow and Pressure Modules

Pressure Control Modules

Auxiliary Pressure Controllers

Advanced User Guide

Carrier Gas Flow Rates

Advanced User Guide

Columns and Oven

Configuring the Oven

Advanced User Guide

Advanced User Guide

Advanced User Guide

Advanced User Guide

Advanced User Guide

Service Reminders 400 Other functions 401

Advanced User Guide

Advanced User Guide

Agilent 7890A Gas Chromatograph Advanced User Guide

Run Time Programming

Using run time events

Advanced User Guide

Programming run time events

[Enter] after each entry.

The run table

Adding events to the run table

while on the Time: line of any entry.

numbers; others require [On/Yes] or [Off/No].

automatically placed in order by execution time.

Editing events in the run table

labeled Time:. Type the desired time and press [Enter].

Advanced User Guide

Deleting run time events

[Off/No] to cancel this operation.

Advanced User Guide

Clock Time Programming

Using clock time events

Programming clock time events

Adding events to the clock table

automatically ordered chronologically.

Advanced User Guide

Editing clock time events

labelled Time: and type the desired time.

[On/Yes] or [Off/No], or enter a numerical value for the setpoint.

Deleting clock time events

You will be asked to confirm the deletion.

Advanced User Guide

To program a User Key

keystrokes are stored.

To play back (execute) the stored keystrokes

To erase the stored keystrokes

Advanced User Guide

Advanced User Guide

Agilent 7890A Gas Chromatograph Advanced User Guide